Apparatus and method for preparing fluorine-containing oxadiazole

Abstract

The application relates to the field of organic synthesis, in particular to a preparation device and method of fluorine-containing oxadiazole. The device is a rotary evaporator, a hollow tube for steam flow of the rotary evaporator is connected with an evaporating flask, the hollow tube drives the evaporating flask to rotate, and the evaporating flask is partially arranged in a water bath kettle; a bottle withdrawing mechanism is arranged on the rotary evaporator, and the bottle withdrawing mechanism can drive the evaporating flask to rotate and move along the hollow tube axis direction. In the application, the evaporating flask can be quickly fixed by the mode that the rotating ring b extrudes the rotating frame, subsequent rotary evaporation work is facilitated, after the rotary evaporation is completed, the bottle withdrawing mechanism can quickly break the stuck state of the evaporating flask, in the whole operation process, an operator does not need to hold the evaporating flask and rotate and pull it with force, but only needs to rotate the rotating lever a and the rotating lever b, the operation is more labor-saving, the evaporating flask and the water bath kettle will not collide due to excessive force, and the evaporating flask is indirectly protected.

Description

Technical Field

[0001] This invention relates to the field of organic synthesis technology, and in particular to an apparatus and method for preparing fluorinated oxadiazoles. Background Technology

[0002] Fluorinated diazoles are a class of organic compounds with specific chemical structures. These compounds exhibit unique physical, chemical, and biological properties and have important applications in fields such as medicine, pesticides, and materials science. The preparation of fluorinated diazoles requires the use of a rotary evaporator for vacuum distillation to quickly remove large amounts of solvents, such as methanol and ethanol, after the reaction.

[0003] In rotary evaporators, the bottom of the evaporation flask is placed inside a water bath, and the top is fitted onto the rotating shaft. The evaporation flask is then secured with clamps. After use, the evaporation flask needs to be manually removed. However, due to atmospheric pressure, thermal expansion, and solvent residue causing a "seizing" phenomenon, the evaporation flask is difficult to remove. Manually rotating and dragging it outwards is strenuous and carries the risk of the evaporation flask colliding with the water bath. For example, in a filtration method and device for liquid polycarbosilane disclosed in Chinese Patent No. CN114870494B, the evaporation flask is not easily removed manually. Summary of the Invention

[0004] The purpose of this invention is to address the problems in the prior art, such as the difficulty in removing the evaporation flask and the risk of collision between the evaporation flask and the water bath, by proposing a preparation device and method for fluorinated oxadiazole.

[0005] On the one hand, the present invention proposes a preparation device for fluorinated dioxadiazole, specifically a rotary evaporator. The rotary evaporator has a hollow tube for steam flow connected to an evaporation flask. The rotation of the hollow tube drives the evaporation flask to rotate, and the evaporation flask is placed in a water bath. The rotary evaporator is equipped with a flask removal mechanism, which can drive the evaporation flask to rotate and push the evaporation flask to move along the axis of the hollow tube.

[0006] Preferably, the rotary evaporator includes a main unit that drives the hollow tube to rotate and lift, a condenser tube connected to the hollow tube, and a water bath for heating the evaporation flask; the condenser tube is provided with two cooling liquid circulation pipes and a vacuum pipe, a spiral cooling pipe is provided inside the condenser tube, a discharge pipe is provided at the bottom of the condenser tube, a receiving bottle is connected to the discharge pipe, the condenser tube is connected to the feeding pipe through a connecting pipe, and a valve is provided on the feeding pipe.

[0007] Preferably, a fixed outer shell is provided on the main unit, a hollow tube passes through the fixed outer shell, and a cylinder is provided on the side of the fixed outer shell facing the water bath.

[0008] Preferably, the bottle ejection mechanism includes a threaded cylinder a that is threadedly connected to the cylinder body, a rotating ring a that is rotatably disposed on the end face of the threaded cylinder a, a threaded cylinder b that is fitted onto the threaded cylinder a and threadedly engaged, a rotating ring b that is rotatably disposed at the end of the threaded cylinder b, and a rotating frame that is rotatably disposed on the end face of the rotating ring a.

[0009] Preferably, multiple rotating levers a are arranged radially on the outer wall of the threaded cylinder b, and multiple rotating levers b are arranged radially on the outer wall of the rotating ring b.

[0010] Preferably, a support rod is provided at the end of the rotating frame, and a fixed plate is provided on the end face of the rotating ring a. The support rod is rotatably connected to the fixed plate, and a torsion spring is sleeved on the support rod. The two ends of the torsion spring are respectively connected to the rotating frame and the fixed plate.

[0011] Preferably, an arc-shaped protrusion is provided on the outer side of the rotating frame, and multiple elastic pressure plates are provided in the clamping section of the rotating frame. The elastic pressure plates press on the ground joint of the evaporating flask. When the rotating ring b contacts the arc-shaped protrusion, the elastic pressure plates limit the evaporating flask. After the threaded cylinder b continues to move downward until the arc-shaped protrusion moves into the rotating ring b, the elastic pressure plates are further squeezed, thereby increasing the friction between them and the evaporating flask.

[0012] Preferably, a baffle is provided on the outside of the rotating frame, and multiple baffles are provided on the end face of the rotating ring b facing the evaporation flask. When the rotating ring b continues to rotate, the baffles push the baffles, thereby driving the multiple rotating frames to rotate.

[0013] On the other hand, the present invention proposes a method for preparing fluorinated diazoles, comprising the following steps:

[0014] S1. Transfer the reaction mixture into the evaporating flask and place the evaporating flask over the hollow tube;

[0015] S2. Rotate the threaded cylinder b to move the rotating ring b downwards. The rotating ring b contacts the arc-shaped protrusion, so that the elastic pressure plate on the rotating frame initially presses on the ground joint of the evaporating flask to fix the evaporating flask.

[0016] S3. Vacuuming: Under reduced pressure, the solvent is evaporated by heating in a water bath and rotating the evaporation flask by rotating the hollow tube. The evaporated solvent is condensed and falls into the receiving flask for recovery. The residue in the evaporation flask is the concentrated crude product.

[0017] S4. Slowly open the valve to break the vacuum state, rotate the threaded cylinder b to push the rotating ring b to continue to move downwards, and the rotating ring b further squeezes the arc-shaped protrusion so that the elastic pressure plate is tightly pressed against the ground joint of the evaporator flask.

[0018] S5. Continue to rotate the threaded cylinder b, push the baffle through the stop rod, thereby causing the rotating frame to rotate. The rotating frame drives the evaporating flask to rotate, breaking the jammed state of the evaporating flask. Continue to rotate the threaded cylinder b to drive the threaded cylinder a to move downward, causing the evaporating flask to move downward a certain distance.

[0019] S6. Reset the bottle ejection mechanism, remove the evaporation flask, and pour out the crude product. The crude product will then be further processed.

[0020] Compared with the prior art, the present invention has the following beneficial technical effects: the evaporation flask can be quickly fixed by squeezing the rotating frame with the rotating ring b, which facilitates subsequent rotary evaporation. After rotary evaporation, the rotating threaded cylinder b further squeezes the arc-shaped protrusion through the rotating ring b, causing the elastic pressure plate to further squeeze the ground joint of the evaporation flask. Rotating the rotating ring b can then break the jamming state of the evaporation flask. Then, rotating the threaded cylinder b drives the threaded cylinder a to move down synchronously, causing the evaporation flask to move down a short distance, resetting the flask removal mechanism, and removing the evaporation flask. During the entire operation, the operator does not need to hold the evaporation flask and rotate and pull it with force. It is only necessary to rotate the lever a and the lever b. The operation is more labor-saving and will not cause the evaporation flask to collide with the water bath due to excessive force, thus indirectly protecting the evaporation flask. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of the structure of one embodiment of the present invention;

[0022] Figure 2 for Figure 1 A structural diagram from another perspective;

[0023] Figure 3 for Figure 1 Partial structural diagram;

[0024] Figure 4 To fix the relevant structure of the evaporation flask;

[0025] Figure 5 for Figure 4 A schematic diagram of the structure after removing the threaded cylinder b and the rotating ring b;

[0026] Reference numerals: 1. Main unit; 2. Hollow tube; 3. Condenser tube; 4. Vacuum tube; 5. Coolant circulation tube; 6. Discharge tube; 7. Receiving bottle; 8. Evaporating flask; 9. Water bath; 10. Feeding tube; 11. Valve; 12. Fixed outer shell; 13. Cylinder; 14. Threaded cylinder a; 15. Rotating ring a; 16. Rotating frame; 17. Arc-shaped protrusion; 18. Baffle; 19. Elastic pressure plate; 20. Fixed plate; 21. Torsion spring; 22. Threaded cylinder b; 23. Rotating lever a; 24. Rotating ring b; 25. Rotating lever b; 26. Stop bar; 27. Connecting tube. Detailed Implementation

[0027] Example 1; as Figures 1-3As shown, the present invention proposes a preparation device for fluorinated dioxadiazoles, specifically a rotary evaporator. The rotary evaporator has a hollow tube 2 for steam flow connected to an evaporating flask 8. Rotation of the hollow tube 2 causes the evaporating flask 8 to rotate, and the evaporating flask 8 is partially placed inside a water bath 9. The rotary evaporator is equipped with a flask removal mechanism, which rotates the evaporating flask 8 and pushes it along the axis of the hollow tube 2. Specifically, after the work is completed, the evaporating flask 8 is first rotated by the flask removal mechanism to release its jammed state. Then, the evaporating flask 8 is slowly pushed downwards along the axis of the hollow tube 2, at which point it is completely separated from the hollow tube 2 and can be easily removed. This eliminates the need for the operator to forcefully grip and rotate the evaporating flask 8, making the operation more labor-saving and preventing the evaporating flask 8 from colliding with the water bath 9 due to excessive force.

[0028] Example 2; as Figures 1-2 As shown, this invention proposes a preparation device for fluorinated diazoles. Compared to Example 1, this example details the structure of a rotary evaporator. Specifically, the rotary evaporator includes a main unit 1 that drives the hollow tube 2 to rotate and move up and down, a condenser tube 3 connected to the hollow tube 2, and a water bath 9 for heating the evaporation flask 8. The condenser tube 3 is equipped with two cooling liquid circulation pipes 5 and a vacuum pipe 4. A spiral cooling pipe is installed inside the condenser tube 3, and a discharge pipe 6 is installed at the bottom of the condenser tube 3. A receiving bottle 7 is connected to the discharge pipe 6. The condenser tube 3 is connected to the feeding pipe 10 via a connecting pipe 27. A valve 11 is installed on the feeding pipe 10. The vacuum state can be broken simply by rotating the valve 11. Except for the bottle ejection mechanism, the other structures are those found in conventional rotary evaporators, and the technology is relatively mature, so they will not be described in detail here.

[0029] Furthermore, a fixed outer shell 12 is provided on the main unit 1, the hollow tube 2 passes through the fixed outer shell 12, and a cylinder 13 is provided on the side of the fixed outer shell 12 facing the water bath 9. The fixed outer shell 12 is fixed and does not rotate, while the hollow tube 2 and the fixed outer shell 12 rotate relative to each other.

[0030] Example 3; as Figures 3-5 As shown, the present invention proposes a preparation device for fluorinated diazoles. Compared with Embodiment 2, this embodiment details the structure of the bottle ejection mechanism. Specifically, the bottle ejection mechanism includes a threaded cylinder a14 threadedly connected to the cylinder body 13, a rotating ring a15 rotatably disposed on the end face of the threaded cylinder a14, a threaded cylinder b22 sleeved on the threaded cylinder a14 and threadedly engaged, a rotating ring b24 rotatably disposed at the end of the threaded cylinder b22, and a rotating frame 16 rotatably disposed on the end face of the rotating ring a15. When the threaded cylinder b22 rotates downward, the rotating ring b24 presses the rotating frame 16 to press it against the ground joint of the evaporation flask 8, thereby achieving rapid fixation of the evaporation flask 8.

[0031] Furthermore, multiple rotating levers a23 are arranged radially on the outer wall of the threaded cylinder b22, and multiple rotating levers b25 are arranged radially on the outer wall of the rotating ring b24. The threaded cylinder b22 and the rotating ring b24 can be easily rotated by rotating levers a23 and rotating levers b25.

[0032] Furthermore, a support rod is provided at the end of the rotating frame 16, and a fixed plate 20 is provided on the end face of the rotating ring a15. The support rod is rotatably connected to the fixed plate 20. A torsion spring 21 is sleeved on the support rod. The two ends of the torsion spring 21 are respectively connected to the rotating frame 16 and the fixed plate 20. After the threaded cylinder b22 moves upward, under the action of the torsion spring 21, the rotating frame 16 flips outward, which can release the restriction on the evaporation bottle 8, thereby removing the evaporation bottle 8. In an optional embodiment, three rotating frames 16 are provided, and the three rotating frames 16 are evenly distributed in the circumferential direction with the axis of the hollow tube 2 as the center.

[0033] Furthermore, an arc-shaped protrusion 17 is provided on the outer side of the rotating frame 16, and multiple elastic pressure plates 19 are provided on the clamping section of the rotating frame 16. The elastic pressure plates 19 press on the ground joint of the evaporating flask 8. When the rotating ring b24 contacts the arc-shaped protrusion 17, the elastic pressure plates 19 limit the evaporating flask 8. After the threaded cylinder b22 continues to move downward until the arc-shaped protrusion 17 moves into the rotating ring b24, the elastic pressure plates 19 are further squeezed, thereby increasing the friction between them and the evaporating flask 8.

[0034] Furthermore, a baffle 18 is provided on the outer side of the rotating frame 16, and multiple baffles 26 are provided on the end face of the rotating ring b24 facing the evaporating flask 8. When the rotating ring b24 continues to rotate, the baffles 26 push the baffle 18, thereby driving the multiple rotating frames 16 to rotate. Then, through the tight contact between the elastic pressure plate 19 and the evaporating flask 8, the evaporating flask 8 is driven to rotate, releasing the jammed state of the evaporating flask 8. Then, the threaded cylinder b22 continues to move downward until the rotating ring b24 abuts against the baffle 18. The threaded cylinder b22 then rotates. Due to the restriction of the baffle 18, The threaded cylinder b22 will drive the threaded cylinder a14 to rotate together. The downward movement of the threaded cylinder a14 will drive the evaporating flask 8 to move downward a certain distance. This distance can further ensure that the evaporating flask 8 and the hollow tube 2 are completely separated from the tight contact state. After the threaded cylinder b22 is rotated upward, the rotating frame 16 will automatically flip upward, and the evaporating flask 8 can be easily removed. It should be noted that when the threaded cylinder b22 moves upward, in order to prevent the threaded cylinder a14 from moving upward at the same time and bringing the evaporating flask 8 up, you can hold the rotating frame 16 with your hand to keep the threaded cylinder a14 from rotating.

[0035] Example 4; The present invention proposes a method for preparing fluorinated oxadiazoles, using the equipment for preparing fluorinated oxadiazoles as described in Example 3, specifically including the following steps:

[0036] S1. Transfer the reaction mixture into the evaporating flask 8 and place the evaporating flask 8 onto the hollow tube 2;

[0037] S2. Rotate the threaded cylinder b22 to move the rotating ring b24 downward. The rotating ring b24 contacts the arc-shaped protrusion 17, so that the elastic pressure plate 19 on the rotating frame 16 initially presses on the ground joint of the evaporating flask 8 to fix the evaporating flask 8. It should be noted that the initial fixation of the evaporating flask 8 does not require too much clamping force, because after vacuuming, under the action of external atmospheric pressure, the evaporating flask 8 will form a tight contact with the hollow tube 2 and rotate with the hollow tube 2.

[0038] S3. Vacuuming: Under reduced pressure, the solvent is evaporated by heating in a water bath and rotating the evaporating flask 8 by rotating the hollow tube 2. The evaporated solvent is condensed and falls into the receiving flask 7 for recovery. The residue in the evaporating flask 8 is the concentrated crude product.

[0039] S4. Slowly open valve 11 to break the vacuum state. Rotate threaded cylinder b22 to push rotating ring b24 to continue moving downward. Rotating ring b24 further squeezes arc-shaped protrusion 17 so that elastic pressure plate 19 is tightly pressed against the ground joint of evaporating bottle 8.

[0040] S5. Continue rotating the threaded cylinder b22, which pushes the baffle 18 through the stop rod 26, thereby causing the rotating frame 16 to rotate. The rotating frame 16 drives the evaporating flask 8 to rotate, breaking the jammed state of the evaporating flask 8. Continue rotating the threaded cylinder b22 to drive the threaded cylinder a14 to move downward, causing the evaporating flask 8 to move downward a certain distance. It should be noted that if the threaded cylinder a14 moves downward before the rotating ring a15 rotates when rotating the threaded cylinder b22 downward, it means that the connection between the evaporating flask 8 and the hollow tube 2 is not very tight. In this case, there is no need to try rotating the evaporating flask 8 again, because the downward movement of the threaded cylinder a14 has already pushed the evaporating flask 8 downward.

[0041] S6. Reset the bottle ejection mechanism, remove the evaporation flask 8, and pour out the crude product. The crude product will then be further processed.

[0042] In summary, in this invention, the evaporating flask 8 can be quickly fixed by pressing the rotating frame 16 with the rotating ring b24, which facilitates subsequent rotary evaporation. After rotary evaporation, the rotating threaded cylinder b22 further presses the arc-shaped protrusion 17 through the rotating ring b24, causing the elastic pressure plate 19 to further press the ground joint of the evaporating flask 8. Then, rotating the rotating ring b24 can break the jammed state of the evaporating flask 8. Next, rotating the threaded cylinder b22 drives the threaded cylinder a14 to move down synchronously, causing the evaporating flask 8 to move down a small distance, resetting the flask removal mechanism, and removing the evaporating flask 8. During the entire operation, the operator does not need to hold the evaporating flask 8 and rotate and pull it forcefully. It is only necessary to rotate the lever a23 and the lever b25. The operation is more labor-saving and will not cause the evaporating flask 8 to collide with the water bath 9 due to excessive force, thus indirectly protecting the evaporating flask 8.

[0043] The embodiments of the present invention have been described in detail above with reference to the accompanying drawings. However, the present invention is not limited thereto. Various changes can be made within the scope of knowledge possessed by those skilled in the art without departing from the spirit of the present invention.

Claims

1. A device for preparing fluorinated diazole, specifically a rotary evaporator, wherein a hollow tube (2) for steam flow in the rotary evaporator is connected to an evaporation flask (8), the rotation of the hollow tube (2) drives the evaporation flask (8) to rotate, and part of the evaporation flask (8) is placed in a water bath (9); characterized in that, The rotary evaporator is equipped with a bottle removal mechanism, which can drive the evaporating flask (8) to rotate and push the evaporating flask (8) to move along the axis of the hollow tube (2). The bottle removal mechanism includes a threaded cylinder a (14) that is threaded to the cylinder body (13), a rotating ring a (15) that is rotatably set on the end face of the threaded cylinder a (14), a threaded cylinder b (22) that is fitted on the threaded cylinder a (14) and threadedly engaged, a rotating ring b (24) that is rotatably set on the end face of the threaded cylinder b (22), and a rotating frame (16) that is rotatably set on the end face of the rotating ring a (15). An arc-shaped protrusion (17) is provided on the outside of the rotating frame (16). Multiple elastic pressure plates (19) are provided on the clamping section of the rotating frame (16). The elastic pressure plates (19) press on the ground joint of the evaporating flask (8). When the rotating ring b (24) contacts the arc-shaped protrusion (17), the elastic pressure plates (19) press on the ground joint of the evaporating flask (8). 19) Limit the evaporating flask (8). The threaded cylinder b (22) continues to move downward until the arc protrusion (17) moves into the rotating ring b (24). The elastic pressure plate (19) is further squeezed, thereby increasing the friction between it and the evaporating flask (8). A baffle (18) is set on the outside of the rotating frame (16). Multiple baffles (26) are set on the end face of the rotating ring b (24) facing the evaporating flask (8). When the rotating ring b (24) continues to rotate, the baffles (26) push the baffles (18), thereby driving multiple rotating frames (16) to rotate. A support rod is set at the end of the rotating frame (16). A fixed plate (20) is set on the end face of the rotating ring a (15). The support rod is rotatably connected to the fixed plate (20). A torsion spring (21) is sleeved on the support rod. The two ends of the torsion spring (21) are connected to the rotating frame (16) and the fixed plate (20) respectively.

2. The equipment for preparing fluorinated diazoles according to claim 1, characterized in that, The rotary evaporator includes a main unit (1) that drives the hollow tube (2) to rotate and lift, a condenser tube (3) connected to the hollow tube (2), and a water bath (9) for heating the evaporation flask (8); the condenser tube (3) is provided with two cooling liquid circulation pipes (5) and a vacuum pipe (4), the condenser tube (3) is provided with a spiral cooling pipe, the bottom of the condenser tube (3) is provided with a discharge pipe (6), the discharge pipe (6) is connected to a receiving bottle (7), the condenser tube (3) is connected to the feeding pipe (10) through the connecting pipe (27), and the feeding pipe (10) is provided with a valve (11).

3. The equipment for preparing fluorinated diazoles according to claim 1, characterized in that, A fixed outer shell (12) is provided on the main unit (1), and a hollow tube (2) passes through the fixed outer shell (12). A cylinder (13) is provided on the side of the fixed outer shell (12) facing the water bath (9).

4. The equipment for preparing fluorinated diazoles according to claim 1, characterized in that, Multiple rotating levers a (23) are arranged radially on the outer wall of the threaded cylinder b (22), and multiple rotating levers b (25) are arranged radially on the outer wall of the rotating ring b (24).

5. A method for preparing fluorinated oxadiazoles, using the equipment for preparing fluorinated oxadiazoles as described in claim 1, characterized in that, Includes the following steps: S1. Transfer the reaction mixture into the evaporating flask (8) and place the evaporating flask (8) onto the hollow tube (2); S2. Rotate the threaded cylinder b (22) to move the rotating ring b (24) downward. The rotating ring b (24) contacts the arc-shaped protrusion (17), so that the elastic pressure plate (19) on the rotating frame (16) initially presses on the ground joint of the evaporating bottle (8) to fix the evaporating bottle (8). S3. Vacuuming is performed. Under reduced pressure, the solvent is heated by a water bath and rotated by the rotation of the hollow tube (2) to make the solvent evaporate. The evaporated solvent is condensed and falls into the receiving bottle (7) for recovery. The residue in the evaporating bottle (8) is the concentrated crude product. S4. Slowly open the valve (11) to break the vacuum state, rotate the threaded cylinder b (22) to push the rotating ring b (24) to continue to move downward, and the rotating ring b (24) further squeezes the arc-shaped protrusion (17) so that the elastic pressure plate (19) is tightly pressed on the ground joint of the evaporating bottle (8); S5. Continue to rotate the threaded cylinder b (22), push the baffle (18) through the stop bar (26), thereby causing the rotating frame (16) to rotate. The rotating frame (16) drives the evaporating bottle (8) to rotate, breaking the jammed state of the evaporating bottle (8). Continue to rotate the threaded cylinder b (22) to drive the threaded cylinder a (14) to move downward, so that the evaporating bottle (8) moves downward a certain distance. S6. Reset the bottle ejection mechanism, remove the evaporation flask (8), and pour out the crude product. The crude product will then be further processed.

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