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Method for preparing benzisoxazole antipsychotic drug risperidone

An antipsychotic drug, benzoisoxazole technology, applied in the field of preparation of risperidone, can solve the problems of high impurity control requirements, difficult industrialization, harsh conditions, etc., and achieve high product purity, low cost, and small environmental impact Effect

Inactive Publication Date: 2015-04-29
REYOUNG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN101328173, CN101353347, and CN101245065 have carried out special research reports on the above-mentioned impurities respectively, but the above-mentioned impurities control requirements are relatively high, the conditions are relatively harsh, the requirements are relatively high in the actual operation process, and it is difficult to realize industrialization

Method used

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  • Method for preparing benzisoxazole antipsychotic drug risperidone
  • Method for preparing benzisoxazole antipsychotic drug risperidone
  • Method for preparing benzisoxazole antipsychotic drug risperidone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 32ml of 40wt% potassium hydroxide and 48ml of dichloromethane into a 250ml three-necked flask, and add (z)-[3-[4-[(2,4-difluorophenyl)methoximino]piperidinyl ]-1-ethyl]-2-methyl-6,7,8,9-4H-pyrido[1,2-a]pyrimidin-4-one 15g, stirred, heated to 38°C, heated to reflux for 2h, When the reaction system changed from turbid to clear, the reaction was continued for 1 hour, liquid separation, washing, crystallization, and drying were performed to obtain 12.30 g of risperidone. The purity of the obtained risperidone was 99.83%, the mono-impurity was 0.035%, and the yield was 86.03%.

Embodiment 2

[0029] Add 32ml of 35wt% potassium hydroxide and 32ml of dichloromethane into a 250ml three-necked flask, and add (z)-[3-[4-[(2,4-difluorophenyl)methoximino]piperidinyl ]-1-ethyl]-2-methyl-6,7,8,9-4H-pyrido[1,2-a]pyrimidin-4-one 15g, stirred, heated to 41°C, heated to reflux for 3h, When the reaction system changed from turbid to clear, the reaction was continued for 1 hour, liquid separation, washing, crystallization, and drying were performed to obtain 12.65 g of risperidone. The obtained risperidone had a purity of 99.88%, a monotonicity of 0.042%, and a yield of 88.45%.

Embodiment 3

[0031] Add 32ml of 40wt% sodium hydroxide and 64ml of dichloromethane into a 250ml three-necked flask, and add (z)-[3-[4-[(2,4-difluorophenyl)methoximino]piperidinyl ]-1-ethyl]-2-methyl-6,7,8,9-4H-pyrido[1,2-a]pyrimidin-4-one 15g, stirred, heated to 39°C, heated to reflux for 1.5h , when the reaction system changed from turbid to clear, the reaction was continued for 0.5h, liquid separation, washing, crystallization, and drying were performed to obtain 12.40 g of risperidone. The obtained risperidone had a purity of 99.84%, a mono-impurity of 0.041%, and a yield of 86.76%.

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Abstract

The invention relates to a method for preparing a benzisoxazole antipsychotic drug risperidone and belongs to the technical field of preparation of risperidone. The method for preparing a benzisoxazole antipsychotic drug risperidone comprises the following step of carrying out cyclization reaction on (z)-[3-[4-[(2,4-difluorophenyl)methyloximido]piperidinyl]-1-ethyl]-2-methyl-6,7,8,9-4H-pyridino[1,2-a]pyrimidin-4-one serving as a starting material in a mixed solvent of dichloromethane and concentrated alkali water to prepare the target product risperidone. The method is simple in operation and low in requirements on the device, the prepared product is high in purity and is suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of risperidone, a benzisoxazole antipsychotic drug, and belongs to the technical field of risperidone preparation. Background technique [0002] The benzisoxazole antipsychotic drug risperidone is a new generation antipsychotic drug, which has a high affinity with 5-HT2 receptor and dopamine D2 receptor. Its structural formula is as formula (I): [0003] [0004] At present, there are mainly two methods for synthesizing risperidone, namely, the first cyclization and then halogenation route mentioned in US4804663, and the first halogenation and then cyclization route mentioned in EP0368388. Since the specific synthesis method of risperidone is not disclosed in the patent EP0368388, risperidone is mainly synthesized according to the method disclosed in US4804663 in China at present, but a key intermediate 6-fluoro-3-(4-piperidone is involved in this method. The cyclization reaction of pyridyl)-1,2-benzis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 赵玉山许鹏飞李广杨祥龙
Owner REYOUNG PHARMA
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