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Preparation process of perphenazine

A technology of preparation process and process steps, which is applied in the field of preparation of antipsychotic drugs, can solve the problems of low yield, and achieve the effects of high quality, complete reaction and high solubility

Active Publication Date: 2017-07-21
BEIJING JINGFENG PHARM (SHANDONG) CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The yield of traditional preparation method is low

Method used

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  • Preparation process of perphenazine

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Experimental program
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Effect test

Embodiment 1、2

[0037] The preparation technology of embodiment 1,2 and comparative example 1,2

[0038] 1) Synthesis of side chains: Put the mixed solvent / toluene and N-(2-hydroxyethyl)piperazine into the reaction kettle in turn and heat up to 70°C and stir evenly; then cool down to 38°C, add 1,3-bromo Chloropropane reacted for 3.7 hours, cooled and centrifuged to shake off the material;

[0039] 2) Condensation: Put the mixed solvent / toluene, 2-chlorophenothiazine, and sodium hydroxide into the reaction kettle and reflux and dehydrate at 120°C for 3.5 hours; use chloropropyl N-(2-hydroxyethyl)piperazine Add chloropropyl N-(2-hydroxyethyl)piperazine in the form of benzene solution, separate the generated water through the water separator during the dropwise addition, and reflux for 4.5 hours; after cooling to below 100°C, add water and stir Static layering, the alkali water layer is separated to obtain the condensation product;

[0040] 3) Crude product: the condensation product is washed ...

Embodiment 5

[0047] The preparation technology of embodiment 5,6

[0048] 1) Synthesis of side chains: Put the mixed solvent and N-(2-hydroxyethyl)piperazine into the reaction kettle in turn and heat up to 74°C and stir evenly; then cool down to 40°C, add 1,3-bromochloropropane dropwise React for 3.7 hours, cool down, and centrifuge to shake off the material;

[0049] 2) Condensation: Put the mixed solvent, 2-chlorophenothiazine, and sodium hydroxide into the reaction kettle and reflux and dehydrate at 118°C for 4 hours; Add chloropropyl N-(2-hydroxyethyl)piperazine in the form of the solution, separate the generated water through the water separator during the dropwise addition, and reflux for 4 hours; cool down to below 100°C, add water and stir, and then separate Layer, the alkali water layer is separated to obtain the condensation product;

[0050] 3) Crude product: the condensation product is washed successively by adding water, standing for stratification, dividing the water layer ...

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Abstract

The invention discloses a preparation process of perphenazine and belongs to the field of antipsychotics preparation. The preparation process is characterized by including steps: using methylbenzene and xylene as solvents for side chain synthesis, and performing condensation reaction in the solvents quickly; subjecting a condensation product to water washing, acid pickling, alkali washing and hot water washing, heating for distillation, and crystallizing to obtain a crude product; putting acetone, the crude product and activated carbon into a reaction kettle, and heating for backflow; pressing material liquid into a crystallization kettle through a filter; crystallizing and drying to obtain perphenazine. Reaction time of side chain synthesis is shortened to 4h from 6h of conventional processes, and reaction is more complete. The drying process is shortened to 2h from 4h of the conventional processes. Yield of the preparation process is increased to higher than 40% from 21% of the conventional processes.

Description

technical field [0001] The invention discloses a preparation process of perphenazine, which belongs to the field of preparation of antipsychotic drugs. Background technique [0002] Perphenazine is an antipsychotic western medicine. It is mainly a sedative and sleeping medicine, and it has a certain control effect in the treatment of mental illness. The preparation process of traditional perphenazine is: [0003] 1) Side chain synthesis: Put the prepared toluene and hydroxypiperidine into the reaction tank, start stirring to adjust the bath temperature in the tank to make the temperature reach about 50°C, stir the material evenly, and drop it from the high-level bottle when the internal temperature is adjusted to 35°C Add 1,3-bromochloropropane, strictly control the reaction temperature between 35-38°C during the dropwise addition, and not exceed 38°C, and the 1,3-bromochloropropane will be in the form of a line when it is dropped, and the maximum per hour should not exceed...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D279/28
Inventor 司继伟李传龙张克明张隽许桂普
Owner BEIJING JINGFENG PHARM (SHANDONG) CO LTD
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