Resolution device and method for chiral intermediate of formoterol
By designing the splitting device of formoterol chiral intermediate, using a filter and a telescopic cleaning mechanism, the problem of difficulty in filtering and cleaning during recrystallization in the prior art is solved, and the raw materials are fully stirred and cleaned. Improves reaction efficiency and cleaning effect.
Patent Information
- Application Number
- CN202410987510.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-23
- Publication Date
- 2024-12-20
- Estimated Expiration
- Not applicable · inactive patent
AI Technical Summary
The existing formoterol chiral intermediate separation method cannot achieve filtration during recrystallization, and the cleaning of the stirring mechanism is difficult, making cleaning blind spots prone to occur.
A splitting device formoterol chiral intermediate is designed, including recrystallization tank, stirring mechanism and telescopic cleaning mechanism. The raw materials are filtered through the filter screen and two sets of stirring shafts and telescopic cleaning mechanism are used to achieve fullness of the raw materials. Stir and clean, reduce friction and avoid cleaning blind spots.
The full filtration and stirring of raw materials are achieved, the reaction efficiency is improved, and the friction is reduced through the telescopic cleaning mechanism, which improves the cleaning effect of the device.
Smart Images
Figure CN119158292A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of chemical synthesis, in particular to a device and a method for splitting a formoterol chiral intermediate. Background Art
[0002] Formoterol is a long-acting selective adrenergic β2 receptor agonist with bronchodilator effect. It is used to treat dyspnea caused by airway obstructive diseases such as bronchial asthma, chronic tracheitis, asthmatic bronchitis, emphysema, etc. It is especially suitable for patients who need to take adrenergic β2 receptor agonists for a long time and patients with nocturnal asthma.
[0003] After searching, the patent application number CN201210541344.4 proposes a method for splitting a chiral intermediate of formoterol, using diethyl ether, isopropyl ether, a mixed solvent of diethyl ether and isopropyl ether in any proportion, a mixed solvent A or a mixed solvent B for recrystallization, wherein the mixed solvent A is composed of 1 part by volume of methanol or ethanol and 10-100 parts by volume of diethyl ether or isopropyl ether, and the mixed solvent B is composed of 1 part by volume of methanol or ethanol, 1 part by volume of acetone and 10-15 parts by volume of water. After analysis, the above-mentioned prior art needs to be recrystallized during the splitting, and the existing recrystallization is carried out in a test tube, and filtration cannot be achieved during the recrystallization process.
[0004] Therefore, we propose a device and method for splitting formoterol chiral intermediates. Summary of the invention
[0005] The purpose of the present invention is to provide a device and method for splitting a chiral intermediate of formoterol, which solves the problems raised in the background technology.
[0006] The present application embodiment provides a device for separating a chiral intermediate of formoterol, comprising: A recrystallization tank body, a tank cover is installed on the top of the recrystallization tank body, a stirring mechanism is installed inside the recrystallization tank body, a driving mechanism for driving the stirring mechanism to rotate is installed on the top of the tank cover, and a feed joint is provided on the top of the tank cover; A filter screen is slidably mounted on the inner wall of the recrystallization tank body, and a cleaning mechanism for cleaning the filter screen is installed on the stirring mechanism. When the stirring mechanism rotates, the cleaning mechanism can be driven to rotate.
[0007] Preferably, a bracket is fixed to the bottom of the recrystallization tank.
[0008] Preferably, a discharge pipe is provided at the bottom of the recrystallization tank body, a discharge pipe is provided on the side of the discharge pipe, and a valve for controlling the discharge of the discharge pipe is installed on the discharge pipe.
[0009] Preferably, a heating jacket is fixed to the outer wall of the recrystallization tank body, and a liquid inlet and a liquid outlet are provided on the heating jacket, and the liquid inlet is passed through the heating liquid or the cooling liquid.
[0010] Preferably, the stirring mechanism comprises two stirring shafts, the upper ends of the two stirring shafts are linked by a transmission mechanism, the lower ends of the stirring shafts are rotatably mounted on the top of the filter screen through bearings, and stirring blades are installed on the stirring shafts.
[0011] Preferably, the driving mechanism adopts a driving motor.
[0012] Preferably, the cleaning mechanism includes a connecting sleeve, which is fixed on the stirring shaft, a connecting shaft is fixed on one side of the connecting sleeve, a sliding sleeve is movably connected to the end of the connecting shaft, a spring is fixed to the inner wall of the sliding sleeve, the other end of the spring is fixedly connected to the connecting shaft, and bristles are fixed to the bottom of the sliding sleeve and the connecting shaft.
[0013] Preferably, a square opening is formed at the bottom of the sliding sleeve, and the bristles on the connecting shaft are located in the square opening.
[0014] When the stirring mechanism rotates, it can drive the cleaning mechanism to rotate. When the present invention is in use, after the raw materials are added, the raw materials can be filtered through the filter screen, and the raw materials can be fully stirred by the setting of the stirring mechanism, so that the raw materials can fully react. It is worth mentioning that a vertical guide bar is provided on the inner wall of the recrystallization tank body, and a guide groove is provided at the edge of the filter screen, so that the filter screen can extend the guide bar to move vertically, and the guide bar can also limit the filter screen to prevent the filter screen from rotating with the stirring mechanism. The present application adopts two sets of stirring shafts. If an ordinary cleaning mechanism is used, it is bound to cause the problem of cleaning dead corners. In order to solve this problem, the present invention adopts a retractable cleaning mechanism. When the end of the sliding sleeve is reached, it can be pressed against the recrystallization tank body to achieve contraction, and then it can continue to rotate. A ball bearing can be provided at the end of the sliding sleeve to reduce the friction between the sliding sleeve and the recrystallization tank body, thereby achieving better cleaning. The present invention has a square opening at the bottom of the sliding sleeve, so that the bristles on the connecting shaft can slide into the square opening to achieve the storage of the bristles, which will not affect the extension and retraction of the cleaning mechanism.
[0015] A method for splitting a formoterol chiral intermediate adopts a device for splitting a formoterol chiral intermediate and comprises the following steps: feeding a raw material into a recrystallization tank through a feed joint, and heating, cooling and recrystallizing the raw material to obtain the formoterol chiral intermediate.
[0016] Compared with the prior art, the technical solution of this application has the following beneficial effects: When the present invention is used, after the raw materials are added, the raw materials can be filtered through the filter screen, and the raw materials can be fully stirred by setting the stirring mechanism, so that the raw materials can fully react; The present invention adopts a retractable cleaning mechanism. When the end of the sliding sleeve is reached, it can contact the recrystallization tank body to achieve contraction and then continue to rotate. A ball bearing can be arranged at the end of the sliding sleeve to reduce the friction between the sliding sleeve and the recrystallization tank body, thereby achieving better cleaning. BRIEF DESCRIPTION OF THE DRAWINGS
[0017] Other features, objects and advantages of the present invention will become more apparent from the detailed description of non-limiting embodiments made with reference to the following drawings: Figure 1 It is a structural schematic diagram of the separation device of the formoterol chiral intermediate of the present invention; Figure 2 It is a front view of the separation device of the formoterol chiral intermediate of the present invention; Figure 3 It is a partial cutaway view of the device for separating the chiral intermediate of formoterol in the present invention; Figure 4 It is a partial schematic diagram of the cleaning mechanism in the present invention; Figure 5 It is a bottom view of the cleaning mechanism in the present invention.
[0018] In the figure: 1. recrystallization tank body; 2. tank cover; 3. feed joint; 4. transmission mechanism; 5. driving mechanism; 6. heating jacket; 601. liquid inlet; 602. liquid outlet; 7. discharge pipe; 8. valve; 9. bracket; 10. stirring shaft; 11. stirring blade; 12. cleaning mechanism; 1201. connecting sleeve; 1202. connecting shaft; 1203. sliding sleeve; 1204. bristles; 1205. square opening; 1206. spring; 13. discharge pipe; 14. filter screen; 15. bearing. DETAILED DESCRIPTION
[0019] See also Figure 1-5 The present invention provides a technical solution: a device for splitting a chiral intermediate of formoterol, comprising: A recrystallization tank body 1, a tank cover 2 is installed on the top of the recrystallization tank body 1, a stirring mechanism is installed inside the recrystallization tank body 1, a driving mechanism 5 for driving the stirring mechanism to rotate is installed on the top of the tank cover 2, and a feed joint 3 is provided on the top of the tank cover 2; A filter screen 14 is slidably mounted on the inner wall of the recrystallization tank body 1, and a cleaning mechanism 12 for cleaning the filter screen 14 is installed on the stirring mechanism. When the stirring mechanism rotates, the cleaning mechanism 12 can be driven to rotate. When the present invention is in use, after the raw materials are added, the raw materials can be filtered through the filter screen 14, and the raw materials can be fully stirred by the setting of the stirring mechanism, so that the raw materials can fully react. It is worth mentioning that a vertical guide bar is arranged on the inner wall of the recrystallization tank body 1, and a guide groove is arranged at the edge of the filter screen 14, so that the filter screen 14 can extend the guide bar to move vertically, and the guide bar can also limit the filter screen 14 to prevent the filter screen 14 from rotating together with the stirring mechanism.
[0020] like Figure 1 and Figure 2 As shown, in a specific embodiment of the present invention, a bracket 9 is fixed to the bottom of the recrystallization tank body 1, and the bracket 9 is used to support the entire recrystallization tank body 1.
[0021] like Figure 1-Figure 3 As shown, in a specific embodiment of the present invention, a discharge pipe 7 is provided at the bottom of the recrystallization tank body 1, a discharge pipe 13 is provided on the side of the discharge pipe 7, and a valve 8 for controlling the discharge of the discharge pipe 13 is installed on the discharge pipe 7. When the formoterol chiral intermediate is generated, the valve 8 is opened to discharge the product from the discharge pipe 13.
[0022] like Figure 1-Figure 3 As shown, in a specific embodiment of the present invention, a heating jacket 6 is fixed to the outer wall of the recrystallization tank body 1, and a liquid inlet 601 and a liquid outlet 602 are provided on the heating jacket 6. The liquid inlet 601 is passed with a heating liquid or a cooling liquid. When the raw material needs to be heated, the heating liquid is passed, and when the raw material needs to be cooled, the cooling liquid is passed. In this way, the raw material can be quickly heated or cooled to achieve recrystallization of the raw material.
[0023] like Figure 3 As shown, in a specific embodiment of the present invention, the stirring mechanism includes two stirring shafts 10, the upper ends of the two stirring shafts 10 are linked by a transmission mechanism 4, and the lower ends of the stirring shafts 10 are rotatably installed on the top of the filter 14 through a bearing 15, and a stirring blade 11 is installed on the stirring shaft 10. It is worth noting that the transmission mechanism adopts belt drive or gear drive, which can realize the simultaneous rotation of the two stirring shafts 10, so that the raw materials can be stirred at multiple positions, and sufficient mixing can be achieved, and then sufficient reaction can be achieved, and the lower end of the stirring shaft 10 is rotatably installed, so that when the tank cover 2 is opened, the filter 14 can also be taken out at the same time, so that the filter 14 can be cleaned.
[0024] like Figure 1As shown, in a specific embodiment of the present invention, the driving mechanism 5 adopts a driving motor. When the driving motor is running, it drives one of the stirring shafts 10 to rotate, and then drives the other stirring shaft 10 to rotate through the transmission mechanism 4, and the stirring blades 11 fully stir the raw materials.
[0025] like Figure 4 and Figure 5 As shown, in a specific embodiment of the present invention, the cleaning mechanism 12 includes a connecting sleeve 1201, the connecting sleeve 1201 is fixed on the stirring shaft 10, a connecting shaft 1202 is fixed on one side of the connecting sleeve 1201, a sliding sleeve 1203 is movably sleeved at the end of the connecting shaft 1202, a spring 1206 is fixed to the inner wall of the sliding sleeve 1203, the other end of the spring 1206 is fixedly connected to the connecting shaft 1202, bristles 1204 are fixed to the bottom of the sliding sleeve 1203 and the connecting shaft 1202, and when the present invention is in use, after the raw materials are continuously filtered, impurities are bound to clog the filter screen 14, and the stirring shaft 10 During stirring, the cleaning mechanism can also be driven to rotate, so that the bristles 1204 can clean the surface of the filter 14 to avoid clogging and poor filtering effect. In addition, since the present application uses two sets of stirring shafts 10, if an ordinary cleaning mechanism 12 is used, it will inevitably cause the problem of cleaning dead corners. In order to solve this problem, the present invention uses a retractable cleaning mechanism 12. When the end of the sleeve 1203 is reached, it can be pressed against the recrystallization tank body 1 to achieve contraction, and then continue to rotate. A ball bearing can be set at the end of the sleeve 1203 to reduce the friction between the sleeve 1203 and the recrystallization tank body 1, thereby achieving better cleaning.
[0026] like Figure 4 and Figure 5 As shown, in a specific embodiment of the present invention, a square opening portion 1205 is opened at the bottom of the sliding sleeve 1203, and the bristles 1204 on the connecting shaft 1202 are located in the square opening portion 1205. Since the cleaning mechanism 12 needs to be telescopic, but the bristles 1204 cannot be telescopic, if they are arranged side by side, the bristles 1204 on the connecting shaft 1202 will not be able to be retracted into the sliding sleeve 1203, thereby causing the problem that the telescopic mechanism 12 cannot be retracted. The present invention has a square opening portion 1205 at the bottom of the sliding sleeve 1203, so that the bristles 1204 on the connecting shaft 1202 can slide into the square opening portion 1205, so that the bristles 1204 can be stored, and the telescopic mechanism 12 will not be affected.
[0027] A method for splitting a formoterol chiral intermediate adopts a device for splitting a formoterol chiral intermediate, comprising the following steps: feeding a raw material into a recrystallization tank 1 through a feed joint 3, and obtaining a formoterol chiral intermediate after the raw material is heated, cooled and recrystallized.
[0028] Working principle: when the stirring mechanism rotates, it can drive the cleaning mechanism 12 to rotate. When the present invention is in use, after the raw materials are added, the raw materials can be filtered through the filter screen 14, and the raw materials can be fully stirred by the setting of the stirring mechanism, so that the raw materials can be fully reacted. It is worth mentioning that a vertical guide bar is provided on the inner wall of the recrystallization tank body 1, and a guide groove is provided at the edge of the filter screen 14, so that the filter screen 14 can extend the guide bar to move vertically, and the guide bar can also limit the filter screen 14 to prevent the filter screen 14 from rotating together with the stirring mechanism. The present application adopts two sets of stirring shafts 10. If an ordinary cleaning The cleaning mechanism 12 is bound to cause the problem of cleaning dead corners. In order to solve this problem, the present invention adopts a retractable cleaning mechanism 12. When the end of the sleeve 1203 is reached, it can be pressed against the recrystallization tank body 1 to achieve contraction, and then can continue to rotate. A ball bearing can be set at the end of the sleeve 1203 to reduce the friction between the sleeve 1203 and the recrystallization tank body 1, thereby achieving better cleaning. The present invention has a square opening portion 1205 at the bottom of the sleeve 1203, so that the bristles 1204 on the connecting shaft 1202 can slide into the square opening portion 1205 to achieve the storage of the bristles 1204, which will not affect the extension and retraction of the cleaning mechanism 12.
Claims
1. A device for separating chiral intermediates of formoterol, characterized in that: include: A recrystallization tank body (1), a tank cover (2) is installed on the top of the recrystallization tank body (1), a stirring mechanism is installed inside the recrystallization tank body (1), a driving mechanism (5) for driving the stirring mechanism to rotate is installed on the top of the tank cover (2), and a feed joint (3) is provided on the top of the tank cover (2); A filter screen (14) is slidably mounted on the inner wall of the recrystallization tank body (1), and a cleaning mechanism (12) for cleaning the filter screen (14) is mounted on the stirring mechanism. When the stirring mechanism rotates, the cleaning mechanism (12) can be driven to rotate.
2. The device for separating a chiral intermediate of formoterol according to claim 1, characterized in that: A bracket (9) is fixed to the bottom of the recrystallization tank (1).
3. The device for separating a chiral intermediate of formoterol according to claim 1, characterized in that: A discharge pipe (7) is arranged at the bottom of the recrystallization tank body (1), a discharge pipe (13) is arranged on the side of the discharge pipe (7), and a valve (8) for controlling the discharge of the discharge pipe (13) is installed on the discharge pipe (7).
4. The device for separating a chiral intermediate of formoterol according to claim 1, characterized in that: A heating jacket (6) is fixed to the outer wall of the recrystallization tank body (1), and a liquid inlet (601) and a liquid outlet (602) are provided on the heating jacket (6), and a heating liquid or a cooling liquid is introduced into the liquid inlet (601).
5. The device for separating a chiral intermediate of formoterol according to claim 4, characterized in that: The stirring mechanism comprises two stirring shafts (10), the upper ends of the two stirring shafts (10) are linked via a transmission mechanism (4), the lower ends of the stirring shafts (10) are rotatably mounted on the top of the filter screen (14) via bearings (15), and stirring blades (11) are mounted on the stirring shafts (10).
6. The device for separating a chiral intermediate of formoterol according to claim 1, characterized in that: The driving mechanism (5) adopts a driving motor.
7. The device for separating a chiral intermediate of formoterol according to claim 5, characterized in that: The cleaning mechanism (12) comprises a connecting sleeve (1201), wherein the connecting sleeve (1201) is fixed on the stirring shaft (10), a connecting shaft (1202) is fixed on one side of the connecting sleeve (1201), a sliding sleeve (1203) is movably sleeved at the end of the connecting shaft (1202), a spring (1206) is fixed to the inner wall of the sliding sleeve (1203), the other end of the spring (1206) is fixedly connected to the connecting shaft (1202), and bristles (1204) are fixed to the bottom of the sliding sleeve (1203) and the connecting shaft (1202).
8. The device for separating a chiral intermediate of formoterol according to claim 7, characterized in that: A square opening (1205) is formed at the bottom of the sliding sleeve (1203), and the bristles (1204) on the connecting shaft (1202) are located in the square opening (1205).
9. A method for resolving a chiral intermediate of formoterol, characterized in that: The device for splitting the chiral intermediate of formoterol according to claim 8 comprises the following steps: feeding the raw material into the recrystallization tank (1) through the feed connector (3); and obtaining the chiral intermediate of formoterol after the raw material is heated, cooled and recrystallized.