Preparation process and processing equipment of stable sitafloxacin intermediate

Abstract

The invention relates to the technical field of chemical medicine preparation, and discloses stable sitafloxacin intermediate processing equipment which comprises a box body, a bottom shell is fixedly connected to the bottom of the inner wall of the box body, and a cooling mechanism used for separating out a sitafloxacin intermediate from a solution is arranged in the bottom shell. A mixing mechanism for fully mixing a sitafloxacin intermediate solution is arranged at the top of the box body and comprises a motor, the motor is fixedly connected to the top of the box body, a threaded column is fixedly connected to an output shaft of the motor, and a limiting pipe is fixedly connected to the top wall of an inner cavity of the box body; the sitafloxacin intermediate solution in the container is cooled through the second heat conduction pipe, so that the sitafloxacin intermediate in the solution is crystallized and separated out, the stirring rod is still in a continuous rotating state in the process, heat in the solution is evenly distributed, local overheating or supercooling is avoided, crystals are dispersed in the solution, the agglomeration phenomenon is prevented, and the stability of the sitafloxacin intermediate solution is improved. Therefore, the uniformity and the quality of crystallization are improved.

Description

Technical Field

[0001] The invention relates to the technical field of chemical drug preparation, in particular to a preparation process and processing equipment of a stable sitafloxacin intermediate. Background Art

[0002] Sitafloxacin intermediates refer to intermediates or chemical substances produced in the process of synthesizing sitafloxacin. Sitafloxacin is a broad-spectrum quinolone antibacterial drug used to treat various infectious diseases. Intermediates are usually produced at a certain stage in the drug synthesis process. They undergo a series of chemical reactions and processing steps and are ultimately converted into sitafloxacin.

[0003] The specific structure and properties of sitafloxacin intermediates may vary depending on the synthesis route and process. These intermediates play a key role in the drug synthesis process and may require further reaction, purification and transformation to obtain the final sitafloxacin product.

[0004] In order to obtain a stable sitafloxacin intermediate, conventional processing equipment needs to process the intermediate multiple times in multiple steps, wherein the preparation of a saturated solution of the sitafloxacin intermediate and the crystallization of the sitafloxacin intermediate need to be performed step by step, which undoubtedly increases the complexity of preparing the sitafloxacin intermediate, thereby reducing the production efficiency of sitafloxacin, and is not conducive to the rapid production of sitafloxacin. In addition, during the preparation of the sitafloxacin intermediate, the sitafloxacin intermediate needs to be crystallized and precipitated. However, during the crystallization process, due to uneven mixing of the solution and the interaction force between ions during crystallization, the crystals aggregate with each other to form agglomerates, resulting in different sizes of the formed sitafloxacin intermediate crystals, which is not convenient for subsequent processing of the sitafloxacin intermediate.

[0005] To this end, a preparation process and processing equipment of a stable sitafloxacin intermediate are proposed. Summary of the invention

[0006] The object of the present invention is to provide a preparation process and processing equipment of a stable sitafloxacin intermediate to solve the problems raised in the above background technology.

[0007] To achieve the above object, the present invention provides the following technical solution: a stable processing equipment for sitafloxacin intermediates, comprising a box, the bottom of the inner wall of the box is fixedly connected to a bottom shell, the bottom of the bottom shell is provided with a cooling mechanism for precipitating the sitafloxacin intermediate from a solution, and the top of the box is provided with a mixing mechanism for fully mixing a solution containing the sitafloxacin intermediate;

[0008] The mixing mechanism includes a motor, which is fixedly connected to the top of the box body, a threaded column is fixedly connected to the output shaft of the motor, a limiting tube is fixedly connected to the top wall of the inner cavity of the box body, a movable column is slidably connected to the inside of the limiting tube, a sliding member is fixedly connected to the top of the movable column, the sliding member is slidably connected to the inside of the limiting tube, the threaded column is threadedly connected to the inside of the movable column, a stirring rod is rotatably connected to the outside of the movable column, a supporting spring is fixedly connected between the stirring rod and the movable column, a cover is slidably connected to the outside of the limiting tube, and a fixing plate is fixedly connected to the bottom end of the limiting tube The top of the fixed plate is fixedly connected with a return spring, the top of the return spring is fixedly connected to the bottom of the cover body, the bottom of the fixed plate is rotatably connected to a rotating part, the inside of the rotating part is fixedly connected with a spring 1, one end of the spring 1 close to the center point of the rotating part is fixedly connected with a plug plate, the plug plate is slidably connected to the inside of the rotating part, the bottom end of the movable column is fixedly connected with a spring telescopic rod, the bottom end of the spring telescopic rod is rotatably connected to the bottom plate, the top wall of the inner cavity of the box body is rotatably connected with a transmission part 1, and the upper and lower ends of the transmission part 1 are respectively meshed with the top of the threaded column and the outside of the rotating part.

[0009] Furthermore, the mixing mechanism includes a worm gear, which is rotatably connected to the inside of the bottom shell, the top of the worm gear is fixedly connected to a transmission gear, the inside of the bottom shell is slidably connected to two tooth plates, the tops of the two tooth plates are fixedly connected to a positioning plate, the transmission gear is located between the two tooth plates, and the transmission gear is meshed with the two tooth plates at the same time, the top of the bottom shell is slidably connected to a pressing piece, the bottom of the pressing piece is fixedly connected to an ejection spring, the inside of the bottom shell is fixedly connected to a connecting spring located below the pressing piece, and the bottom surface of the pressing piece and the top of the connecting spring are both An electrode is fixedly connected, a refrigerator is fixedly connected to the bottom of the box, a heat conduction pipe 1 is fixedly connected to the top of the refrigerator, a heat conduction pipe 2 is fixedly connected to the inside of the positioning plate, an end of the heat conduction pipe 2 close to the refrigerator is fixedly connected to a connecting pipe and is communicated with the connecting pipe, an end of the connecting pipe away from the positioning plate is fixedly connected to a one-way valve, an impeller is rotatably connected to the inside of the connecting pipe, and a transmission member 2 and a transmission member 3 are rotatably connected to the inner wall of the box, the ends of the transmission member 2 and the transmission member 3 that are close to each other are meshed with each other, and the ends of the transmission member 2 and the transmission member 3 that are away from each other are meshed with the transmission member 1 and the impeller respectively.

[0010] Furthermore, a groove is provided at the top of the outer side of the movable column, and limiting grooves are provided on the four sides of the limiting tube. Four support rods are fixedly connected to the top of the sliding member, and the four support rods are slidably connected to the four limiting grooves respectively.

[0011] Furthermore, four blocks are fixedly connected to the inner wall of the cover body, and the four blocks are slidably connected to four limiting grooves, and the side of the plug plate close to the movable column is in contact with the stirring rod.

[0012] Furthermore, the two electrodes are connected in series with the refrigerator, the top end of the pressing member passes through the bottom shell, the positioning plate is arc-shaped, and the heat pipe 2 is coiled and passes through the interior of the positioning plate.

[0013] Furthermore, the connecting pipe is connected to the heat conducting pipe 2, the bottom end of the transmission member 3 passes through the connecting pipe, and the connection between the transmission member 3 and the connecting pipe is sealed.

[0014] Furthermore, one end of the connecting pipe close to the one-way valve passes through the box, the inner wall of the box is fixedly connected to an insulation board, the outer wall of the connecting pipe is in contact with heat conducting pipe 1, and the connecting pipe and heat conducting pipe 1 are both located inside the insulation board.

[0015] The preparation process of a stable sitafloxacin intermediate comprises the following steps:

[0016] Step 1: preparing raw materials, wherein the raw materials include 2,4-diamino-6-chloropyridine, chloroacetamide and boric acid;

[0017] Step 2: Under dry conditions, reacting 2,4-diamino-6-chloropyridine with chloroacetamide to generate N-acetyl-2,4-diamino-6-chloropyridine intermediate;

[0018] Step 3: condense the N-acetyl-2,4-diamino-6-chloropyridine intermediate with boric acid to generate a sitafloxacin intermediate. The factors involved in the reaction, such as the selection of solvent, reaction time and temperature, need to be adjusted according to specific experimental conditions.

[0019] Step 4: Select a solvent that can dissolve the target compound but does not chemically react with the target compound, and dissolve the target compound in an appropriate amount of the solvent until the solution no longer dissolves more target compound;

[0020] Step 5: refrigerate the saturated solution in a refrigerator or freezer to lower the temperature of the solution, thereby reducing the solubility of the target compound in the solution, thereby causing the target compound crystals to precipitate;

[0021] Step 6: Filter the crystallized solution through a filter to separate the crystals and the remaining solution, and finally dry the filtered crystals in a dryer to remove the residual solvent;

[0022] Step 7: Use appropriate analytical instruments to identify and quantify the intermediates to ensure that the quality of the intermediates meets the requirements.

[0023] Compared with the prior art, the present invention has the following beneficial effects:

[0024] First, the container containing the sitafloxacin intermediate solution is clamped and positioned by two positioning plates and the bottom plate presses the bottom of the inner wall of the container to prevent the container from shifting or even tipping over when the device mixes the solution in the container, thereby improving the use effect of the device. At the same time, the cover body covers the top of the container to prevent the solution from splashing during the mixing process, thereby ensuring the cleanliness of the inside of the box and preventing the waste of the solution.

[0025] The stirring rod can rotate continuously inside the container to stir the solution containing the sitafloxacin intermediate, so that the reactants in the solution are fully mixed, avoiding the situation of local excessively high or low concentration, and increasing the contact area between the reactants, thereby accelerating the reaction rate. At the same time, since the stirring rod is connected to the movable column through a supporting spring, the stirring rod will vibrate up and down during the rotation process, thereby accelerating the exchange speed of the upper and lower parts of the solution and further improving the solution mixing effect.

[0026] Secondly, the sitafloxacin intermediate solution in the container is cooled by the second heat conducting pipe so that the sitafloxacin intermediate in the solution is crystallized and precipitated. During this process, the stirring rod is still in a state of continuous rotation, so that the heat in the solution is evenly distributed, local overheating or overcooling is avoided, and the crystals are dispersed in the solution to prevent the occurrence of agglomeration, thereby improving the uniformity and quality of the crystallization. At the same time, the mixing and crystallization steps of preparing the sitafloxacin intermediate can be carried out simultaneously by stirring and cooling, which simplifies the preparation steps of the sitafloxacin intermediate, thereby improving the production and processing efficiency of the sitafloxacin intermediate and realizing rapid production;

[0027] When the motor output shaft rotates in the reverse direction, the movable column and the stirring rod can be reset, and the impeller can be rotated in the reverse direction, and the cold air inside the heat transfer pipe 2 is transported to the outside through the one-way valve, so as to avoid the residual cold air in the heat transfer pipe 2 lowering the solution temperature when the sitafloxacin intermediate solution is mixed by the device again, so as to prevent the sitafloxacin intermediate from being unable to be completely dissolved due to the lowering of the solution temperature, thereby improving the use effect of the device and facilitating the repeated use of the device. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the overall structure of the present invention;

[0029] Figure 2 It is a schematic cross-sectional view of the overall structure of the present invention;

[0030] Figure 3 It is a cross-sectional schematic diagram of the bottom shell structure of the present invention;

[0031] Figure 4 This is a schematic diagram of the installation of the transmission gear structure of the present invention;

[0032] Figure 5 This is a schematic diagram of the installation of the impeller structure of the present invention;

[0033] Figure 6 It is a schematic cross-sectional view of the movable column structure of the present invention;

[0034] Figure 7 For the present invention Figure 6 A schematic diagram of the structure enlargement in the middle;

[0035] Figure 8 This is a schematic diagram of the installation of the rotating part structure of the present invention.

[0036] In the figure:

[0037] 1. Box body; 11. Bottom shell;

[0038] The mixing mechanism includes: 201, motor; 202, threaded column; 203, limit tube; 204, sliding member; 205, movable column; 206, stirring rod; 207, supporting spring; 208, cover body; 209, return spring; 210, fixed plate; 211, rotating member; 212, spring 1; 213, plug plate; 214, spring telescopic rod; 215, bottom plate; 216, transmission member 1;

[0039] The cooling mechanism includes: 301, worm wheel; 302, transmission gear; 303, worm; 304, tooth plate; 305, positioning plate; 306, pressing part; 307, electrode; 308, ejection spring; 309, connecting spring; 310, refrigerator; 311, heat transfer pipe 1; 312, heat transfer pipe 2; 313, connecting pipe; 314, one-way valve; 315, impeller; 316, transmission part 2; 317, transmission part 3. DETAILED DESCRIPTION

[0040] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0041] Embodiment 1

[0042] See also Figures 1 to 8 As shown, an embodiment of the present invention provides: a stable processing equipment for sitafloxacin intermediates, comprising a box body 1, a bottom shell 11 is fixedly connected to the bottom of the inner wall of the box body 1, a cooling mechanism for precipitating the sitafloxacin intermediate from the solution is arranged inside the bottom shell 11, and a mixing mechanism for fully mixing the solution containing the sitafloxacin intermediate is arranged on the top of the box body 1;

[0043] The mixing mechanism includes a motor 201, which is fixedly connected to the top of the box body 1, and a threaded column 202 is fixedly connected to the output shaft of the motor 201. A limit tube 203 is fixedly connected to the top wall of the inner cavity of the box body 1, and a movable column 205 is slidably connected inside the limit tube 203. A sliding member 204 is fixedly connected to the top of the movable column 205, and the sliding member 204 is slidably connected to the inside of the limit tube 203. The threaded column 202 is threadedly connected to the inside of the movable column 205. A stirring rod 206 is rotatably connected to the outside of the movable column 205, and a supporting spring 207 is fixedly connected between the stirring rod 206 and the movable column 205. A cover body 208 is slidably connected to the outside of the limit tube 203, and a fixed plate 210 is fixedly connected to the bottom end of the limit tube 203. The top of the fixed plate 210 is fixedly connected with a return spring 209, the top of the return spring 209 is fixedly connected to the bottom of the cover body 208, the bottom of the fixed plate 210 is rotatably connected with a rotating member 211, the interior of the rotating member 211 is fixedly connected with a spring 212, one end of the spring 212 close to the center point of the rotating member 211 is fixedly connected with a plug plate 213, the plug plate 213 is slidably connected to the interior of the rotating member 211, the bottom end of the movable column 205 is fixedly connected with a spring telescopic rod 214, the bottom end of the spring telescopic rod 214 is rotatably connected with a bottom plate 215, the top wall of the inner cavity of the box body 1 is rotatably connected with a transmission member 216, the upper and lower ends of the transmission member 216 are respectively meshed with the top of the threaded column 202 and the outside of the rotating member 211.

[0044] Furthermore, the mixing mechanism includes a worm gear 301, which is rotatably connected to the inside of the bottom shell 11, a transmission gear 302 is fixedly connected to the top of the worm gear 301, two tooth plates 304 are slidably connected to the inside of the bottom shell 11, and the tops of the two tooth plates 304 are fixedly connected to positioning plates 305, the transmission gear 302 is located between the two tooth plates 304, and the transmission gear 302 is meshed with the two tooth plates 304 at the same time, a pressing piece 306 is slidably connected to the top of the bottom shell 11, and an ejection spring 308 is fixedly connected to the bottom of the pressing piece 306, and a connecting spring 309 located below the pressing piece 306 is fixedly connected to the inside of the bottom shell 11, and the bottom surface of the pressing piece 306 and the top of the connecting spring 309 are fixedly connected Electrode 307, the bottom of the box 1 is fixedly connected to a refrigerator 310, the top of the refrigerator 310 is fixedly connected to a heat conduction pipe 1 311, the interior of the positioning plate 305 is fixedly connected to a heat conduction pipe 2 312, the end of the heat conduction pipe 2 312 close to the refrigerator 310 is fixedly connected to a connecting pipe 313 and communicated with the same, the end of the connecting pipe 313 away from the positioning plate 305 is fixedly connected to a one-way valve 314, the interior of the connecting pipe 313 is rotatably connected to an impeller 315, the inner wall of the box 1 is rotatably connected to a transmission member 2 316 and a transmission member 3 317, the ends of the transmission member 2 316 and the transmission member 3 317 that are close to each other are meshed with each other, and the ends of the transmission member 2 316 and the transmission member 3 317 that are away from each other are meshed with the transmission member 1 216 and the impeller 315 respectively.

[0045] Furthermore, a groove is provided at the top of the outer side of the movable column 205, and limiting grooves are provided on the four sides of the limiting tube 203. Four support rods are fixedly connected to the top of the sliding member, and the four support rods are respectively slidably connected to the four limiting grooves. After the groove is aligned with the plug plate 213, the stretching elastic force of the spring 1 212 drives the plug plate 213 to embed into the groove of the movable column 205. At this time, the rotation of the rotating member 211 can drive the plug plate 213 and the movable column 205 to rotate.

[0046] Furthermore, four blocks are fixedly connected to the inner wall of the cover body, and the four blocks are slidably connected to the four limit grooves. The side of the plug plate 213 close to the movable column 205 is in contact with the stirring rod 206. Since the stirring rod 206 is connected to the movable column 205 through the supporting spring 207, the stirring rod 206 will vibrate up and down during the rotation, thereby accelerating the exchange speed of the upper and lower parts of the solution and further improving the solution mixing effect.

[0047] Furthermore, the two electrodes 307 are connected in series with the refrigerator 310, the top of the pressing piece 306 passes through the bottom shell 11, the positioning plate 305 is arc-shaped, and the heat pipe 312 is coiled and passes through the interior of the positioning plate 305. The container is clamped, fixed and positioned by the two positioning plates 305 to prevent the container from shifting or even tipping over during use, thereby improving the use effect of the device.

[0048] Furthermore, the connecting pipe 313 is connected to the heat-conducting pipe 2 312, the bottom end of the transmission member 317 passes through the connecting pipe 313, the connection between the transmission member 317 and the connecting pipe 313 is sealed, and the rotation of the impeller 315 can circulate the air inside the heat-conducting pipe 2 312, so as to cool the air in the heat-conducting pipe 2 312 through the refrigerator 310 and the heat-conducting pipe 1 311, and at the same time enable the heat-conducting pipe 2 312 to evenly cool the solution.

[0049] Furthermore, one end of the connecting pipe 313 close to the one-way valve 314 passes through the box body 1, and the inner wall of the box body 1 is fixedly connected with an insulation board. The outer wall of the connecting pipe 313 is in contact with the heat conducting pipe 311. The connecting pipe 313 and the heat conducting pipe 311 are both located inside the insulation board. The insulation board is used to insulate the heat conducting pipe 311, thereby saving energy.

[0050] Embodiment 2

[0051] The preparation process of a stable sitafloxacin intermediate comprises the following steps:

[0052] Step 1: preparing raw materials, wherein the raw materials include 2,4-diamino-6-chloropyridine, chloroacetamide and boric acid;

[0053] Step 2: Under dry conditions, reacting 2,4-diamino-6-chloropyridine with chloroacetamide to generate N-acetyl-2,4-diamino-6-chloropyridine intermediate;

[0054] Step 3: condense the N-acetyl-2,4-diamino-6-chloropyridine intermediate with boric acid to generate a sitafloxacin intermediate. The factors involved in the reaction, such as the selection of solvent, reaction time and temperature, need to be adjusted according to specific experimental conditions.

[0055] Step 4: Select a solvent that can dissolve the target compound but does not chemically react with the target compound, and dissolve the target compound in an appropriate amount of the solvent until the solution no longer dissolves more target compound;

[0056] Step 5: refrigerate the saturated solution in a refrigerator or freezer to lower the temperature of the solution, thereby reducing the solubility of the target compound in the solution, thereby causing the target compound crystals to precipitate;

[0057] Step 6: Filter the crystallized solution through a filter to separate the crystals and the remaining solution, and finally dry the filtered crystals in a dryer to remove the residual solvent;

[0058] Step 7: Use appropriate analytical instruments such as NMR, IR, HPLC, etc. to identify and quantify the intermediates to ensure that the quality of the intermediates meets the requirements.

[0059] Working principle: In the initial state, the distance between the two positioning plates 305 is larger than the diameter of the container containing the sitafloxacin intermediate solution, and the support spring 207 and spring 1 212 are in a compressed state;

[0060] When preparing a stable sitafloxacin intermediate, the sitafloxacin intermediate is first poured into the reaction solvent manually, and then the container containing the reaction solvent is placed between the two positioning plates 305. The weight of the container presses the pressing member 306 downward, and the ejection spring 308 is compressed. The pressing member 306 moves and drives the electrode 307 fixed thereto to move downward until the electrode 307 is pressed on another electrode 307. At this time, the two electrodes 307 are in contact, and the connecting spring 309 is compressed by pressure, and the refrigerator 310 is in a state of being connected to the power supply. Through this design, the refrigerator 310 can be automatically started, thereby improving the automation degree of the device, simplifying the operation process, making it easier and more convenient to use, and avoiding The refrigerator 310 runs continuously to achieve the effect of saving energy. The worm 303 is manually rotated, and the rotation of the worm 303 drives the worm wheel 301 to rotate. The rotation of the worm wheel 301 drives the transmission gear 302 to rotate. The rotation of the transmission gear 302 drives the two tooth plates 304 to move in the opposite direction. The two tooth plates 304 move in the opposite direction and drive the two positioning plates 305 to move towards each other, so that the two positioning plates 305 are respectively clamped on both sides of the container to clamp and fix the container, thereby preventing the container from shifting or even tipping over during use of the device, thereby improving the use effect of the device. At the same time, the cover body 208 covers the top of the container to prevent the solution from splashing during mixing, thereby ensuring the cleanliness of the inside of the box body 1 and preventing the solution from being wasted.

[0061] The motor 201 is started manually, and the output shaft of the motor 201 rotates to drive the threaded column 202 and the transmission member 216 to rotate. Under the limit of the limit tube 203, the threaded column 202 rotates to drive the movable column 205 to move downward, and the transmission member 216 rotates to drive the rotating member 211 to rotate, and the rotating member 211 rotates to drive the plug plate 213 to rotate. At this time, since the movable column 205 is limited, the rotation of the plug plate 213 will not drive the movable column 205 to rotate. The movable column 205 moves downward to drive the sliding member 204, the spring telescopic rod 214 and the bottom plate 215 to move downward, and the bottom plate 215 moves downward to extend into the container. When the bottom plate 215 is lowered to contact and press the bottom of the inner wall of the container, the spring telescopic rod 214 is compressed. At this time, the movable column 205 is out of the threaded connection state with the threaded column 202 and the top of the movable column 205 is out of the bottom of the limiting tube 203. Therefore, the threaded column 202 continues to rotate and will no longer drive the movable column 205 to move downward. The groove of the movable column 205 is lowered to the same height as the plug plate 213. The stretching elastic force of the spring 212 drives the plug plate 213 to embed into the groove of the movable column 205. The sliding member 204 is lowered to contact the top of the cover body 208 and lower the cover body 208. The cover 208 is pressed down by the pressure and the return spring 209 is compressed. After the cover 208 is lowered, it covers the top of the container. The output shaft of the motor 201 continues to rotate to drive the transmission member 216 to rotate. The rotation of the transmission member 216 drives the rotating member 211 to rotate. The rotation of the rotating member 211 drives the plug plate 213 to rotate. The rotation of the plug plate 213 drives the movable column 205 to rotate. As the movable column 205 descends, it drives the stirring rod 206 to escape from the inside of the limiting tube 203. After the stirring rod 206 escapes from the inside of the limiting tube 203, the stretching elastic force of the support spring 207 drives the stirring rod 206 to escape from the inside of the limiting tube 203. 6 is unfolded, so the movable column 205 rotates to drive the unfolded stirring rod 206 to rotate, so that the stirring rod 206 rotates continuously inside the container to stir the solution containing the sitafloxacin intermediate, so that the reactants in the solution are fully mixed, avoiding the situation of excessively high or low local concentration, and increasing the contact area between the reactants, thereby accelerating the reaction rate. Since the stirring rod 206 is connected to the movable column 205 through the supporting spring 207, the stirring rod 206 will vibrate up and down during the rotation process, thereby accelerating the exchange speed of the upper and lower parts of the solution, and further improving the solution mixing effect;

[0062] The transmission member 1 216 rotates while driving the transmission member 2 316 to rotate, the transmission member 2 316 rotates and drives the transmission member 3 317 to rotate, and the transmission member 3 317 rotates and drives the impeller 315 to rotate. After the refrigerator 310 is powered on, since the solution inside the container has its own temperature, it takes some time to cool down, and the solutions mix quickly. Therefore, before the temperature of the refrigerator 310 and the heat pipe 1 311 is reduced, the solution inside the container has been mixed evenly. After the refrigerator 310 cools the heat pipe 1 311 to a certain temperature, the impeller 315 rotates to circulate the air inside the heat pipe 2 312. During the air transportation process, the heat pipe 1 311 absorbs the heat in the air, so that the air temperature inside the heat pipe 2 312 is reduced, and the heat pipe 2 311 is cooled. 2. Cooling down the heat of the sitafloxacin intermediate solution in the absorption container, thereby cooling the sitafloxacin intermediate solution. The cooling of the solution causes the crystals of the sitafloxacin intermediate inside to precipitate. During this process, the stirring rod 206 is still in a state of continuous slow rotation. This slow rotation and stirring can make the solution flow slowly, so that the heat in the solution is evenly distributed, avoiding local overheating or overcooling, and dispersing the crystals in the solution to prevent the occurrence of agglomeration, thereby improving the uniformity and quality of crystallization. In addition, the slow flow of the solution will not affect the crystallization of the solution. At the same time, the above design can make the mixing and crystallization of the sitafloxacin intermediate be carried out simultaneously, simplifying the preparation steps of the sitafloxacin intermediate, thereby improving the production and processing efficiency of the sitafloxacin intermediate and realizing rapid production;

[0063] After the sitafloxacin intermediate is precipitated, the output shaft of the motor 201 is manually controlled to rotate in the opposite direction, and the stretching elastic force of the spring telescopic rod 214 drives the movable column 205 to move upward and resume the threaded connection with the threaded column 202, so that the output shaft of the motor 201 rotates in the opposite direction to drive the movable column 205 to move upward and re-enter the interior of the limiting tube 203. Under the squeezing of the limiting tube 203, the stirring rod 206 is closed together on the outside of the movable column 205, and the supporting spring 207 is compressed. At this time, the impeller 315 rotates in the opposite direction to transport the cold air inside the heat transfer pipe 2 312 to the outside through the one-way valve 314, so as to avoid the residual cold air in the heat transfer pipe 2 312 lowering the solution temperature when the sitafloxacin intermediate solution is mixed by this device again, resulting in the inability of the sitafloxacin intermediate to be completely dissolved, thereby improving the use effect of the device and facilitating the repeated use of the device.

[0064] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device. In the absence of further restrictions, the elements defined by the sentence "including one..." do not exclude the existence of other identical elements in the process, method, article or device including the elements.

[0065] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A stable processing device for sitafloxacin intermediates, comprising a housing (1), characterized in that: The bottom of the inner wall of the box (1) is fixedly connected to a bottom shell (11), the bottom shell (11) is provided with a cooling mechanism for allowing the sitafloxacin intermediate to precipitate from the solution, and the top of the box (1) is provided with a mixing mechanism for fully mixing the solution containing the sitafloxacin intermediate; The mixing mechanism comprises a motor (201), wherein the motor (201) is fixedly connected to the top of a housing (1), a threaded column (202) is fixedly connected to the output shaft of the motor (201), a limit tube (203) is fixedly connected to the top wall of the inner cavity of the housing (1), a movable column (205) is slidably connected inside the limit tube (203), a sliding member (204) is fixedly connected to the top of the movable column (205), the sliding member (204) is slidably connected to the inside of the limit tube (203), the threaded column (202) is threadedly connected to the inside of the movable column (205), a stirring rod (206) is rotatably connected to the outside of the movable column (205), a supporting spring (207) is fixedly connected between the stirring rod (206) and the movable column (205), a cover (208) is slidably connected to the outside of the limit tube (203), and a fixed plate (206) is fixedly connected to the bottom of the limit tube (203). 210), the top of the fixed plate (210) is fixedly connected to a return spring (209), the top of the return spring (209) is fixedly connected to the bottom of the cover body (208), the bottom of the fixed plate (210) is rotatably connected to a rotating member (211), the interior of the rotating member (211) is fixedly connected to a spring 1 (212), and one end of the spring 1 (212) close to the center point of the rotating member (211) is fixedly connected to an insert plate (213), The plug plate (213) is slidably connected to the inside of the rotating member (211); the bottom end of the movable column (205) is fixedly connected to a spring telescopic rod (214); the bottom end of the spring telescopic rod (214) is rotatably connected to a bottom plate (215); the top wall of the inner cavity of the box body (1) is rotatably connected to a transmission member 1 (216); the upper and lower ends of the transmission member 1 (216) are respectively meshed with the top end of the threaded column (202) and the outside of the rotating member (211).

2. The processing equipment of a stable sitafloxacin intermediate according to claim 1, characterized in that: The mixing mechanism comprises a worm gear (301), the worm gear (301) is rotatably connected to the inside of the bottom shell (11), the top of the worm gear (301) is fixedly connected to a transmission gear (302), the inside of the bottom shell (11) is slidably connected to two tooth plates (304), the tops of the two tooth plates (304) are fixedly connected to a positioning plate (305), the transmission gear (302) is located between the two tooth plates (304), and the transmission gear (302) is meshedly connected to the two tooth plates (304) at the same time, the top of the bottom shell (11) is slidably connected to a pressing piece (306), the bottom of the pressing piece (306) is fixedly connected to an ejection spring (308), the inside of the bottom shell (11) is fixedly connected to a connecting spring (309) located below the pressing piece (306), and the bottom surface of the pressing piece (306) and the top of the connecting spring (309) are fixedly connected to an electrode (307), the bottom of the box body (1) is fixedly connected to a refrigerator (310), the top of the refrigerator (310) is fixedly connected to a heat conduction pipe 1 (311), the interior of the positioning plate (305) is fixedly connected to a heat conduction pipe 2 (312), one end of the heat conduction pipe 2 (312) close to the refrigerator (310) is fixedly connected to a connecting pipe (313) and communicated therewith, and the end of the connecting pipe (313) away from the positioning plate (305) is fixedly connected to a connecting pipe (313). A one-way valve (314) is connected, the interior of the connecting pipe (313) is rotatably connected to an impeller (315), the inner wall of the box body (1) is rotatably connected to a transmission member 2 (316) and a transmission member 3 (317), the ends of the transmission member 2 (316) and the transmission member 3 (317) that are close to each other are meshed with each other, and the ends of the transmission member 2 (316) and the transmission member 3 (317) that are far away from each other are meshed with the transmission member 1 (216) and the impeller (315) respectively.

3. The processing equipment of a stable sitafloxacin intermediate according to claim 1, characterized in that: The top of the movable column (205) is provided with a groove, the four sides of the limiting tube (203) are provided with limiting grooves, and the top of the sliding member (204) is fixedly connected with four support rods, and the four support rods are respectively slidably connected to the four limiting grooves.

4. The processing equipment of a stable sitafloxacin intermediate according to claim 1, characterized in that: Four blocks are fixedly connected to the inner wall of the cover body (208), and the four blocks are slidably connected to four limit grooves. The side of the plug plate (213) close to the movable column (205) is in contact with the stirring rod (206).

5. The processing equipment of a stable sitafloxacin intermediate according to claim 2, characterized in that: The two electrodes (307) are connected in series with the refrigerator (310), the top end of the pressing member (306) passes through the bottom shell (11), the positioning plate (305) is arc-shaped, and the second heat conduction pipe (312) is coiled and passes through the interior of the positioning plate (305).

6. The processing equipment of a stable sitafloxacin intermediate according to claim 2, characterized in that: The connecting pipe (313) is connected to the second heat conducting pipe (312), the bottom end of the third transmission member (317) passes through the connecting pipe (313), and the connection between the third transmission member (317) and the connecting pipe (313) is sealed.

7. The processing equipment of a stable sitafloxacin intermediate according to claim 2, characterized in that: One end of the connecting pipe (313) close to the one-way valve (314) passes through the box body (1); the inner wall of the box body (1) is fixedly connected to a heat preservation plate; the outer wall of the connecting pipe (313) is in contact with heat conduction pipe one (311); and the connecting pipe (313) and heat conduction pipe one (311) are both located inside the heat preservation plate.

8. A process for preparing a stable sitafloxacin intermediate, applied to a processing device for a stable sitafloxacin intermediate according to any one of claims 1 to 7, characterized in that: The following steps are involved: Step 1: preparing raw materials, wherein the raw materials include 2,4-diamino-6-chloropyridine, chloroacetamide and boric acid; Step 2: Under dry conditions, reacting 2,4-diamino-6-chloropyridine with chloroacetamide to generate N-acetyl-2,4-diamino-6-chloropyridine intermediate; Step 3: condense the N-acetyl-2,4-diamino-6-chloropyridine intermediate with boric acid to generate a sitafloxacin intermediate. The factors involved in the reaction process, such as the selection of solvent, reaction time and temperature, need to be adjusted according to specific experimental conditions; Step 4: Select a solvent that can dissolve the target compound but does not chemically react with the target compound, and dissolve the target compound in an appropriate amount of the solvent until the solution no longer dissolves more target compound; Step 5: refrigerate the saturated solution in a refrigerator or freezer to lower the temperature of the solution, thereby reducing the solubility of the target compound in the solution, thereby causing the target compound crystals to precipitate; Step 6: Filter the crystallized solution through a filter to separate the crystals and the remaining solution, and finally dry the filtered crystals in a dryer to remove the residual solvent; Step 7: Use appropriate analytical instruments to identify and quantify the intermediates to ensure that the quality of the intermediates meets the requirements.

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