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Synthetic method of diphenhydrazide hydrochloride

A technique for the synthesis of trihexyphenidyl hydrochloride and its synthesis method, which is applied in the field of synthesis of trihexyphenidyl hydrochloride, can solve the problems of low yield and difficulty in further improving the purity, and achieve the effects of high safety, increased yield, and improved promotion

Active Publication Date: 2021-03-12
常州康普药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In order to solve the above problems, the present invention provides a synthetic method of trihexyphenidyl hydrochloride, which solves the problems of low yield and difficulty in further improving the purity in traditional techniques

Method used

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  • Synthetic method of diphenhydrazide hydrochloride
  • Synthetic method of diphenhydrazide hydrochloride

Examples

Experimental program
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Embodiment 1

[0027] (1) Put 7.2kg of magnesium flakes, 4.2kg of chlorocyclohexane, 42kg of methyl tetrahydrofuran and 1.3kg of iodoethane into a dry and clean reaction kettle, cover the feeding port of the reaction kettle, stir until the reaction is initiated, and the initiation time 40min;

[0028] (2) After initiating completely, heat to reflux state, then dropwise add the mixed solution of 31.2kg chlorocyclohexane and 25.2kg methyltetrahydrofuran; dropwise, stir and insulate for reflux reaction for 80min;

[0029] (3) Step (2) Continue to keep the reflux state after the heat preservation reaction ends, slowly add 30kg propiophenone piperidine hydrochloride, then insulate and reflux between 75°C for 120min, add water methyl tetrahydrofuran (moisture content) after the heat preservation finishes 1%), stirred and mixed for 10min, and cooled to room temperature, then slowly heated up and distilled to recover the methyl tetrahydrofuran solvent;

[0030] (4) Add 45.6kg mass fraction of 30% h...

Embodiment 2

[0035] (1) Put 8.8kg of magnesium flakes, 5.2kg of chlorocyclohexane, 52kg of methyl tetrahydrofuran and 2.0kg of iodoethane into a dry and clean reaction kettle, cover the feeding port of the reaction kettle, stir until the reaction is initiated, and the initiation time 35min;

[0036] (2) After initiating completely, heat to reflux state, then dropwise add the mixed solution of 41.6kg chlorocyclohexane and 33.4kg methyltetrahydrofuran; After dropwise addition, stir and insulate for reflux reaction for 70min;

[0037] (3) Step (2) Continue to keep the reflux state after the insulation reaction ends, slowly add 40kg propiophenone piperidine hydrochloride, then insulate and reflux between 70°C for 120min, add water methyl tetrahydrofuran (moisture content) after the insulation finishes 1%), stirred and mixed for 10min, and cooled to room temperature, then slowly heated up and distilled to recover the methyl tetrahydrofuran solvent;

[0038] (4) Add 60.8kg mass fraction of 30% ...

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Abstract

The invention provides a synthetic method of diphenhydrazide hydrochloride, which belongs to the field of drug synthesis, and comprises the following steps: mixing and stirring magnesium tablets, chlorocyclohexane, methyltetrahydrofuran and iodoethane until reaction is initiated, heating to a reflux state, dropwisely adding a mixed solution of chlorocyclohexane and methyltetrahydrofuran, heating to reflux state, adding propiophenone piperidine hydrochloride after heat preservation and reflux reaction, collecting and obtaining a crude product of diphenhydrazide hydrochloride through the steps of subsequent treatment and the like, and performing purifying through a mixed solvent to obtain diphenhydrazide. According to the present invention, the diphenesol hydrochloride is prepared from the iodoethane, the chlorocyclohexane and other raw materials, such that the yield of the diphenesol hydrochloride can be easily increased, the methyl tetrahydrofuran is selected as the reaction solvent, the safety is high, and the yield of the diphenesol hydrochloride can be easily increased compared to the traditional ether solvent;isopropanol and acetone are selected as a mixed solvent, so that thepurity of the diphenhydrazide hydrochloride is improved, and the dissolution loss rate of the diphenhydrazide hydrochloride is reduced, so that the yield of the diphenhydrazide hydrochloride is further improved.

Description

technical field [0001] The invention belongs to the field of medicine synthesis and provides a synthesis method of trihexyphenidyl hydrochloride. Background technique [0002] The chemical name of trihexyphenidyl hydrochloride is 1-cyclohexyl-1-phenyl-3-(1-piperidinyl)-propanol hydrochloride, which acts to selectively block the cholinergic neural pathway in the striatum, It has little effect on the periphery, which helps to restore the balance of dopamine and acetylcholine in the brain of patients with Parkinson's disease, and improves the symptoms of Parkinson's disease in patients. However, the existing preparation technology of trihexyphenidyl hydrochloride has always been to prepare intermediate Propiphenone hydrochloride, piperidine hydrochloride and Grignard reagent are polymerized to make trihexyphenidyl hydrochloride, and the Grignard reagent that adopts in the preparation technology of existing trihexyphenidyl hydrochloride all adopts ether as Reaction solvent, but...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D295/092
CPCC07D295/092
Inventor 殷晓伟王姝汤金春
Owner 常州康普药业有限公司
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