Slegiline hydrochloride purification device
By designing a selegiline hydrochloride purification device and adopting extraction, separation, crystallization and decolorization steps, the problem of low purity of crude selegiline hydrochloride was solved, and high-purity and high-quality selegiline hydrochloride production was achieved, which reduced production costs and shortened the cycle.
Patent Information
- Application Number
- CN202422858765.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-21
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2034-11-21
AI Technical Summary
In the existing selegiline hydrochloride production process, the purity of the crude selegiline hydrochloride is not high, which affects the product quality.
A selegiline hydrochloride purification device was designed, which included an extraction tank, a crystallization tank, a filter, a dryer and other components. Through extraction, separation, crystallization, decolorization and other steps, dextrorotatory ephedrine hydrochloride and propidynyl bromide were separated and purified to improve the product purity.
The production of high-purity selegiline hydrochloride is achieved, production costs are reduced, product quality and color are improved, and production cycle is shortened.
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Figure CN223416779U_ABST
Abstract
Description
Technical Field
[0001] The utility model relates to the technical field of selegiline hydrochloride production, in particular to a selegiline hydrochloride purification device. Background Art
[0002] Selegiline hydrochloride is an organic compound with the chemical formula C 13 H 18 ClN is a selective monoamine oxidase-B inhibitor that inhibits dopamine reuptake and presynaptic receptors. These effects promote dopamine function in the brain. In the treatment of early Parkinson's disease, double-blind clinical trials have shown that patients taking ClN alone, without levodopa, maintained significantly longer functional capacity than those in the placebo group, and were able to maintain a high level of work ability. When added to levodopa, ClN can enhance and prolong the effects of levodopa, thereby reducing the levodopa dosage. When used in combination with levodopa, ClN is particularly effective in reducing the fluctuations of Parkinson's disease. Unlike traditional non-selective monoamine oxidase inhibitors, ClN does not increase the hypertensive (cheese effect) reaction of tyramine.
[0003] Currently, the production process of selegiline hydrochloride mostly uses dextrorotatory ephedrine hydrochloride as the starting material, which undergoes a Friedel-Crafts reaction with acetic anhydride to obtain a selegiline acylate, which is then subjected to catalytic hydrogenation to obtain a selegiline reduced product. The reduced product is then reacted with propidium bromide and acidified with hydrochloric acid to obtain a crude selegiline hydrochloride product. However, the crude selegiline hydrochloride product contains unreacted dextrorotatory ephedrine hydrochloride and propidium bromide, resulting in low product purity and affecting product quality. Summary of the Invention
[0004] The technical problem to be solved by the utility model is: in view of the deficiencies in the prior art, a selegiline hydrochloride purification device is provided, and the obtained product has high purity and good quality.
[0005] In order to solve the above technical problems, the technical solution of the utility model is:
[0006] A selegiline hydrochloride purification device comprises an extraction tank connected to a selegiline hydrochloride crude product tank, wherein the inlet of the extraction tank is connected to a purified water tank and an ether tank via pipelines, respectively; the outlet of the extraction tank is connected to an upper liquid tank and a lower liquid tank via pipelines, respectively; the outlet of the lower liquid tank is connected to a first crystallization tank via a pipeline, the outlet of the first crystallization tank is connected to a first filter via a pipeline, the outlet of the first filter is connected to a dextroephedrine hydrochloride collection tank and a selegiline hydrochloride collection tank, respectively; the outlet of the selegiline hydrochloride collection tank is connected to a dryer, and the outlet of the dryer is connected to a selegiline hydrochloride product tank.
[0007] As an improved technical solution, the outlet of the upper liquid tank is connected to a distillation tank through a pipeline, the upper outlet of the distillation tank is connected to a propyne bromide recovery tank, and the lower outlet of the distillation tank is connected to an ether recovery tank.
[0008] As an improved technical solution, the outlet of the ether recovery tank is connected to the inlet of the ether tank through a pipeline.
[0009] As an improved technical solution, the outlet of the lower liquid tank is connected to a static stratification tank through a pipeline, the outlet of the static stratification tank is connected to an organic phase tank and an aqueous phase tank through pipelines respectively, and the outlet of the aqueous phase tank is connected to the first crystallization tank.
[0010] As an improved technical solution, the outlet of the organic phase tank is connected to the distillation tank through a pipeline.
[0011] As an improved technical solution, the outlet of the water phase tank is connected to a decolorization tank through a pipeline, the outlet of the decolorization tank is connected to a second filter, and the outlet of the second filter is connected to the first crystallization tank through a pipeline.
[0012] The outlet of the selegiline hydrochloride collecting tank is connected to a second crystallization tank, and the outlet of the second crystallization tank is connected to the dryer.
[0013] Due to the adoption of the above technical solution, the beneficial effects of the utility model are:
[0014] The utility model discloses a selegiline hydrochloride purification device, comprising an extraction tank connected to a selegiline hydrochloride crude product tank, wherein the inlet of the extraction tank is connected to a purified water tank and an ether tank via pipelines, the outlet of the extraction tank is connected to an upper liquid tank and a lower liquid tank via pipelines, the outlet of the lower liquid tank is connected to a first crystallization tank via a pipeline, the outlet of the first crystallization tank is connected to a first filter via a pipeline, the outlet of the first filter is connected to a dextroephedrine hydrochloride collection tank and a selegiline hydrochloride collection tank, the outlet of the selegiline hydrochloride collection tank is connected to a dryer, and the outlet of the dryer is connected to a selegiline hydrochloride product tank. The crude selegiline hydrochloride product first enters an extraction tank, and then purified water and ether are added. Dextrorotatory ephedrine hydrochloride and selegiline hydrochloride are dissolved in water, while propargyl bromide is dissolved in ether. After layering, the upper liquid and the lower liquid are separated, wherein dextrorotatory ephedrine hydrochloride and selegiline hydrochloride are located in the lower layer. The crude product then enters a first crystallization tank. During the evaporation and crystallization process, dextrorotatory ephedrine hydrochloride is first precipitated. After filtration, selegiline hydrochloride is dried and dehydrated to finally obtain a high-purity selegiline hydrochloride product with high product quality.
[0015] The outlet of the upper liquid tank of the utility model is connected to a distillation tank via a pipeline, the upper outlet of the distillation tank is connected to a propyne bromide recovery tank, and the lower outlet of the distillation tank is connected to an ether recovery tank. The raw material propyne bromide is recovered after extraction and separation, thereby avoiding waste and reducing production costs.
[0016] The outlet of the ether recovery tank is connected to the inlet of the ether tank through a pipeline. The ether after extraction and recovery can be reused as an extraction agent to avoid waste.
[0017] The outlet of the lower layer liquid tank is connected to a static stratification tank via a pipeline, and the outlet of the static stratification tank is connected to an organic phase tank and an aqueous phase tank via pipelines, respectively. The outlet of the aqueous phase tank is connected to the first crystallization tank. The lower layer liquid is subjected to further static separation, which improves the separation effect and increases the purity of the product.
[0018] The outlet of the organic phase tank is connected to the distillation tank through a pipeline. The organic phase obtained by separation can be transferred to the distillation tank for separation and extraction to avoid waste of raw materials.
[0019] The outlet of the aqueous phase tank is connected to a decolorizing tank via a pipeline, the outlet of the decolorizing tank is connected to a second filter, and the outlet of the second filter is connected to the first crystallization tank via a pipeline. Decolorizing the product by the decolorizing tank improves the color of the product and obtains a high-quality product.
[0020] The outlet of the selegiline hydrochloride collecting tank is connected to a second crystallizer, and the outlet of the second crystallizer is connected to the dryer. The selegiline hydrochloride is pre-concentrated in the second crystallizer and then dried in the dryer, thereby shortening the production cycle. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0022] Figure 1 It is a structural schematic diagram of an embodiment of the utility model;
[0023] Among them: 1. Selegiline hydrochloride crude product tank; 2. Extraction tank; 3. Purified water tank; 4. Ether tank; 5. Upper liquid tank; 6. Lower liquid tank; 7. First crystallization tank; 8. First filter; 9. Dextrorotatory ephedrine hydrochloride collection tank; 10. Selegiline hydrochloride collection tank; 11. Dryer; 12. Selegiline hydrochloride product tank; 13. Distillation tank; 14. Propyl bromide recovery tank; 15. Ether recovery tank; 16. Standing stratification tank; 17. Organic phase tank; 18. Aqueous phase tank; 19. Decolorization tank; 20. Second filter; 21. Second crystallization tank. DETAILED DESCRIPTION
[0024] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0025] like Figure 1 As shown, a selegiline hydrochloride purification device includes an extraction tank 2 connected to a selegiline hydrochloride crude product tank 1, the inlet of the extraction tank 2 is connected to a purified water tank 3 and an ether tank 4 through pipelines, the outlet of the extraction tank 2 is connected to an upper liquid tank 5 and a lower liquid tank 6 through pipelines, the outlet of the lower liquid tank 6 is connected to a first crystallization tank 7 through a pipeline, the outlet of the first crystallization tank 7 is connected to a first filter 8 through a pipeline, the outlet of the first filter 8 is connected to a dextroephedrine hydrochloride collecting tank 9 and a selegiline hydrochloride collecting tank 10, the outlet of the selegiline hydrochloride collecting tank 10 is connected to a dryer 11, and the outlet of the dryer 11 is connected to a selegiline hydrochloride product tank 12. The crude selegiline hydrochloride product first enters an extraction tank 2, and then purified water and ether are added. Dextrorotatory ephedrine hydrochloride and selegiline hydrochloride are dissolved in water, while propargyl bromide is dissolved in ether. After layering, the upper liquid and the lower liquid are separated, wherein the dextrorotatory ephedrine hydrochloride and selegiline hydrochloride are located in the lower layer. The crude selegiline hydrochloride then enters a first crystallization tank 7. During the evaporation and crystallization process, dextrorotatory ephedrine hydrochloride is first precipitated. After filtration, the selegiline hydrochloride is dried and dehydrated to finally obtain a high-purity selegiline hydrochloride product with high product quality.
[0026] The outlet of the upper liquid tank 5 is connected to a distillation tank 13 through a pipeline. The upper outlet of the distillation tank 13 is connected to a propyne bromide recovery tank 14, and the lower outlet of the distillation tank 13 is connected to an ether recovery tank 15. The raw material propyne bromide is recovered after extraction and separation, thereby avoiding waste and reducing production costs.
[0027] The outlet of the ether recovery tank 15 is connected to the inlet of the ether tank 4 through a pipeline. The ether recovered by extraction can be reused as an extraction agent to avoid waste.
[0028] The outlet of the lower layer liquid tank 6 is connected to a static stratification tank 16 via a pipeline, and the outlet of the static stratification tank 16 is connected to an organic phase tank 17 and an aqueous phase tank 18 via pipelines, respectively. The outlet of the aqueous phase tank 18 is connected to the first crystallization tank 7. The lower layer liquid is subjected to further static separation, which has a better separation effect and improves the purity of the product.
[0029] The outlet of the organic phase tank 17 is connected to the distillation tank 13 through a pipeline. The organic phase obtained by separation can be transferred to the distillation tank 13 for separation and extraction to avoid waste of raw materials.
[0030] The outlet of the aqueous phase tank 18 is connected to a decolorizing tank 19 via a pipeline, and the outlet of the decolorizing tank 19 is connected to a second filter 20. The outlet of the second filter 20 is connected to the first crystallization tank 7 via a pipeline. The decolorizing tank 19 decolorizes the product, thereby improving the color of the product and obtaining a high-quality product.
[0031] The outlet of the selegiline hydrochloride collecting tank 10 is connected to the second crystallizer 21, and the outlet of the second crystallizer 21 is connected to the dryer 11. The second crystallizer 21 is pre-concentrated and then dried in the dryer 11, which shortens the production cycle.
[0032] It should be understood that these embodiments are intended only to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the contents of the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms also fall within the scope defined by the appended claims of this application.
Claims
1. A selegiline hydrochloride purification device, characterized in that: The invention comprises an extraction tank connected to a selegiline hydrochloride crude product tank, wherein the inlet of the extraction tank is connected to a purified water tank and an ether tank respectively through pipelines, the outlet of the extraction tank is connected to an upper liquid tank and a lower liquid tank respectively through pipelines, the outlet of the lower liquid tank is connected to a first crystallization tank through a pipeline, the outlet of the first crystallization tank is connected to a first filter through a pipeline, the outlet of the first filter is connected to a dextroephedrine hydrochloride collection tank and a selegiline hydrochloride collection tank respectively, the outlet of the selegiline hydrochloride collection tank is connected to a dryer, and the outlet of the dryer is connected to a selegiline hydrochloride product tank.
2. A selegiline hydrochloride purification device as claimed in claim 1, characterized in that: The outlet of the upper liquid tank is connected to a distillation tank through a pipeline, the upper outlet of the distillation tank is connected to a propyne bromide recovery tank, and the lower outlet of the distillation tank is connected to an ether recovery tank.
3. A selegiline hydrochloride purification device as claimed in claim 2, characterized in that: The outlet of the ether recovery tank is connected to the inlet of the ether tank through a pipeline.
4. A selegiline hydrochloride purification device as claimed in claim 2, characterized in that: The outlet of the lower liquid tank is connected to a static stratification tank through a pipeline, and the outlet of the static stratification tank is connected to an organic phase tank and an aqueous phase tank through pipelines respectively, and the outlet of the aqueous phase tank is connected to the first crystallization tank.
5. A selegiline hydrochloride purification device as claimed in claim 4, characterized in that: The outlet of the organic phase tank is connected to the distillation tank through a pipeline.
6. A selegiline hydrochloride purification device as claimed in claim 4, characterized in that: The outlet of the water phase tank is connected to a decolorizing tank through a pipeline, the outlet of the decolorizing tank is connected to a second filter, and the outlet of the second filter is connected to the first crystallization tank through a pipeline.
7. A selegiline hydrochloride purification device as claimed in claim 1, characterized in that: The outlet of the selegiline hydrochloride collecting tank is connected to a second crystallization tank, and the outlet of the second crystallization tank is connected to the dryer.