Reaction device for 5-azaspiro [2.4] heptane and salt thereof

Abstract

According to the reaction device for the 5-azaspiro [2.4] heptane and the salt thereof, the reaction tank and the separation tank are combined into a whole, the reaction liquid after reaction can be directly filtered for solid-liquid separation, and the following steps of washing, suction filtration and the like can be completed in the device and do not need to be transferred; materials to be post-treated are mixed in the reaction tank, are discharged from the first discharge port after being mixed, are uniformly dispersed between the first separation cylinder and the second separation cylinder through the shunting panel, and are filtered in two directions; separated liquid is timely discharged to a discharging cavity through a first flow guide hole and a second flow guide hole and is discharged from a discharging opening of the discharging cavity, the liquid divided by the flow dividing panel impacts a first separation barrel and a second separation barrel, so that solids are deposited to the bottom, and after filtration is finished, the solids are discharged from a slag outlet hole to a slag outlet; the device is simple in structure and easy and convenient to operate, and post-treatment efficiency is improved.

Description

Technical Field

[0001] The invention belongs to the technical field of reaction kettles, and in particular relates to a reaction device for 5-azaspiro[2.4]heptane and a salt thereof. Background Art

[0002] 5-Azaspiro[2.4]heptane (I), as a homologue of tetrahydropyrrole, has been widely used in drug development. Patent CN202110584864.2 provides a method for preparing 5-azaspiro[2.4]heptane and its salt, comprising the following steps: (1) dissolving cyclopropyl nitrile in a first solvent, adding ethylene oxide, and reacting under strong alkaline conditions to obtain 1-(2-hydroxy-ethyl)-cyclopropanecarbonitrile; (2) dissolving 1-(2-hydroxy-ethyl)-cyclopropanecarbonitrile in a second solvent, adding a reducing agent, and reacting to obtain 2-(1-aminomethyl-cyclopropyl)-ethanol; (3) dissolving 2-(1-aminomethyl-cyclopropyl)-ethanol in a third solvent, adding a protecting agent under alkaline conditions to react to obtain 5-(R-)azaspiro[2.4]heptane; (4) dissolving 5-(R-)azaspiro[2.4]heptane in a fourth solvent, adding a deprotecting agent, and then adding an alkaline agent to obtain 5-azaspiro[2.4]heptane or its salt. In this preparation step, washing, filtering and suction solid-liquid separation devices are used many times. Existing devices often use multiple devices to complete the reaction and post-processing, and it is difficult to discharge the material after solid-liquid separation, which affects continuous operation. Summary of the invention

[0003] In order to solve the above problems, the present invention discloses a reaction device for 5-azaspiro[2.4]heptane and its salt.

[0004] To achieve the above object, the technical solution of the present invention is as follows:

[0005] A reaction device for 5-azaspiro[2.4]heptane and its salt comprises a reaction tank and a solid-liquid separation tank which are arranged in sequence from top to bottom, a sealing cover is arranged on the reaction tank, a driving mechanism is arranged at the center of the sealing cover, a feeding port is also arranged on the sealing cover, the driving mechanism is connected to a rotating shaft, the rotating shaft passes through the sealing cover and is placed in the reaction tank, a stirring paddle is arranged at the bottom of the rotating shaft, a lower end of the rotating shaft is placed at the bottom of the reaction tank through a limiting block positioning rod, a first discharge port is arranged at the bottom of the reaction tank, the reaction tank is bolted to the separation tank, a first positioning plate is arranged at the top of the separation tank, the first discharge port passes through the first positioning plate, a second positioning plate is arranged at the bottom of the separation tank, a first separation cylinder is arranged at the center position in the separation tank, a diversion panel is arranged at the top of the first separation cylinder, the bottom of the first separation cylinder is connected to the second positioning plate, a second separation cylinder is arranged outside the first separation cylinder, the top of the second separation cylinder is connected to the first positioning plate, the bottom of the second separation cylinder is connected to the second positioning plate, the bottom of the separation tank is an inverted cone structure, and a slag discharge port is arranged at the bottom of the separation tank.

[0006] Furthermore, the bottom of the reaction tank is in an inverted cone shape, and a solenoid valve is arranged in the first discharge port to facilitate automatic discharge.

[0007] Furthermore, a diversion panel is arranged directly below the first discharge port, and first through holes are evenly arranged on the second separation cylinder, and second through holes are evenly arranged on the second separation cylinder; the diversion panel evenly disperses the liquid between the first separation cylinder and the second separation cylinder, performs solid-liquid separation in both directions, and improves separation efficiency.

[0008] Furthermore, a first guide hole, a second guide hole and a slag discharge hole are arranged on the second positioning plate, a plurality of first guide holes are arranged in the first separation cylinder, a plurality of second guide holes are arranged outside the second separation cylinder, 2-6 slag discharge holes are arranged between the first separation cylinder and the second separation cylinder, and a solenoid valve is arranged in the slag discharge hole; the separated liquid is discharged in time through the first guide hole and the second guide hole, and the liquid diverted by the diversion panel impacts the first separation cylinder and the second separation cylinder, so that the solids are deposited to the bottom, which is convenient for discharge from the slag discharge hole.

[0009] Furthermore, a flow partition corresponding to the second separation cylinder and an isolation groove corresponding to the first separation cylinder are arranged in the inverted cone structure at the bottom of the separation tank, the flow partition groove and the flow partition are connected by multiple pipelines, a discharge cavity is formed between the flow partition and the bottom of the separation tank, and a second discharge port is arranged in the discharge cavity. The liquid discharged in time through the first guide hole and the second guide hole is discharged from the second discharge port of the discharge cavity, and the separated solid is discharged through the slag discharge hole and the slag discharge port.

[0010] The beneficial effects of the present invention are:

[0011] The present invention discloses a reaction device for 5-azaspiro[2.4]heptane and its salt, which combines a reaction tank and a separation tank into one, and the reaction liquid after the reaction can be directly filtered for solid-liquid separation, and subsequent washing, suction filtration and other steps can be completed in the device without transfer. The utility model has a simple structure, is easy to operate, and improves the post-processing efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 It is a schematic diagram of the three-dimensional structure of the utility model;

[0013] Figure 2 This is a schematic diagram of the internal structure of the utility model;

[0014] List of Figure Symbols:

[0015] 1. Reaction tank; 2. Sealing cover; 3. Driving mechanism; 4. Feed inlet; 5. Separation tank; 6. Slag outlet; 7. Rotating shaft; 8. Agitator; 9. Limiting block; 10. First discharge outlet; 11. Diverter panel; 12. First separation cylinder; 13. Second separation cylinder; 14. First positioning plate; 15. Second positioning plate; 16. Second guide hole; 17. Slag outlet; 18. Isolation trough; 19. Discharge cavity; 20. Second discharge outlet. DETAILED DESCRIPTION

[0016] The present invention will be further explained below in conjunction with the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. Example 1

[0017] A reaction device for 5-azaspiro[2.4]heptane and its salts, comprising a reaction tank 1 and a solid-liquid separation tank 5 arranged in sequence from top to bottom, a sealing cover 2 is arranged on the reaction tank 1, a driving mechanism 3 is arranged at the center of the sealing cover 2, a feed port 4 is also arranged on the sealing cover 2, the driving mechanism 3 is connected to a rotating shaft 7, the rotating shaft 7 passes through the sealing cover 2 and is placed in the reaction tank 1, a stirring paddle 8 is arranged at the bottom of the rotating shaft 7, the lower end of the rotating shaft 7 is placed at the bottom of the reaction tank 1 through a limit block 9 and a positioning rod, the bottom of the reaction tank 1 is an inverted cone, a first discharge port 10 is arranged at the bottom of the reaction tank 1, and a solenoid valve is arranged in the first discharge port 10; the reaction tank 1 is bolted to the separation tank 5, a first positioning plate 14 is arranged at the top of the separation tank 5, the first discharge port 10 passes through the first positioning plate 14, and a second positioning plate 14 is arranged at the bottom of the separation tank 5. A first separation cylinder 12 is arranged at the center position in the separation tank 5, a diverter panel 11 is arranged at the top of the first separation cylinder 12, the bottom end of the first separation cylinder 12 is connected to the second positioning plate 15, a second separation cylinder 13 is arranged outside the first separation cylinder 12, the top end of the second separation cylinder 13 is connected to the first positioning plate 14, the bottom end of the second separation cylinder 13 is connected to the second positioning plate 15, the second positioning plate 15 is provided with a first guide hole, a second guide hole 16, and a slag discharge hole 17, a plurality of first guide holes are arranged in the first separation cylinder 12, a plurality of second guide holes 16 are arranged outside the second separation cylinder 13, four slag discharge holes 17 are arranged between the first separation cylinder 12 and the second separation cylinder 13, and a solenoid valve is arranged in the slag discharge hole 17; the bottom of the separation tank 5 is an inverted cone structure, and a slag discharge port 6 is arranged at the bottom of the separation tank 5.

[0018] Directly below the first discharge port 10 is a flow distribution panel 11 , the second separation cylinder 13 is evenly provided with first through holes, and the second separation cylinder 13 is evenly provided with second through holes; the flow distribution panel 11 evenly distributes the liquid between the first separation cylinder 12 and the second separation cylinder 13 .

[0019] A flow partition corresponding to the second separation cylinder 13 and an isolation groove 18 corresponding to the first separation cylinder 12 are arranged in the inverted cone structure at the bottom of the separation tank. The flow partition groove and the flow partition are connected by multiple pipelines. A discharge cavity 19 is formed between the flow partition and the bottom of the separation tank 5. The discharge cavity 19 is provided with a second discharge port 20.

[0020] Working principle: the post-processed materials are mixed in the reaction tank 1, discharged from the first discharge port 10 after mixing, and evenly dispersed between the first separation cylinder 12 and the second separation cylinder 13 through the diverter panel 11, and filtered in both directions; the separated liquid is promptly discharged to the discharge chamber 19 through the first guide hole and the second guide hole 16, and discharged from the discharge port of the discharge chamber 19. The liquid diverted by the diverter panel 11 impacts the first separation cylinder 12 and the second separation cylinder 13, so that the solid is deposited to the bottom, and after the filtration is completed, it is discharged from the slag discharge hole 17 to the slag discharge port 6.

[0021] It should be noted that the above content only illustrates the technical idea of ​​the present invention and cannot be used to limit the protection scope of the present invention. For ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications all fall within the protection scope of the claims of the present invention.

Claims

1. A reaction device for 5-azaspiro[2.4]heptane and its salts, characterized in that: It includes a reaction tank and a solid-liquid separation tank which are arranged in sequence up and down, a sealing cover is arranged on the reaction tank, a driving mechanism is arranged at the center of the sealing cover, a feeding port is also arranged on the sealing cover, the driving mechanism is connected to a rotating shaft, the rotating shaft passes through the sealing cover and is placed in the reaction tank, a stirring paddle is arranged at the bottom of the rotating shaft, the lower end of the rotating shaft is placed at the bottom of the reaction tank through a limiting block positioning rod, a first discharge port is arranged at the bottom of the reaction tank, the reaction tank is bolted to the separation tank, a first positioning plate is arranged at the top of the separation tank, the first discharge port passes through the first positioning plate, a second positioning plate is arranged at the bottom of the separation tank, a first separation cylinder is arranged at the center position in the separation tank, a diversion panel is arranged at the top of the first separation cylinder, the bottom end of the first separation cylinder is connected to the second positioning plate, a second separation cylinder is arranged outside the first separation cylinder, the top end of the second separation cylinder is connected to the first positioning plate, the bottom end of the second separation cylinder is connected to the second positioning plate, the bottom of the separation tank is an inverted cone structure, and a slag discharge port is arranged at the bottom of the separation tank.

2. The reaction device of 5-azaspiro[2.4]heptane and its salt according to claim 1, characterized in that: The bottom of the reaction tank is in an inverted cone shape, and a solenoid valve is arranged in the first discharge port.

3. The reaction device of 5-azaspiro[2.4]heptane and its salt according to claim 1, characterized in that: Directly below the first discharge port is a flow distribution panel, the second separation cylinder is evenly provided with first through holes, and the second separation cylinder is evenly provided with second through holes.

4. The reaction device of 5-azaspiro[2.4]heptane and its salt according to claim 1, characterized in that: The second positioning plate is provided with a first guide hole, a second guide hole and a slag discharge hole, a plurality of first guide holes are provided in the first separation cylinder, a plurality of second guide holes are provided outside the second separation cylinder, 2-6 slag discharge holes are provided between the first separation cylinder and the second separation cylinder, and a solenoid valve is provided in the slag discharge hole.

5. The reaction device of 5-azaspiro[2.4]heptane and its salt according to claim 4, characterized in that: A flow partition corresponding to the second separation cylinder and an isolation groove corresponding to the first separation cylinder are arranged in the inverted cone structure at the bottom of the separation tank. The flow partition groove and the flow partition are connected by multiple pipelines. A discharge cavity is formed between the flow partition and the bottom of the separation tank, and a second discharge port is arranged in the discharge cavity.

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