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Chlorpromazine hydrochloride synthesis process

A kind of technology of chlorpromazine hydrochloride and synthesis technology, applied in the field of synthesis technology of chlorpromazine hydrochloride, can solve the problems such as not very high yield of chlorpromazine hydrochloride, large quality difference, etc., achieve molar yield improvement, improve yield , the effect of improving the molar yield

Active Publication Date: 2013-11-06
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

The yield of above-mentioned synthetic technique gained chlorpromazine hydrochloride is not very high, and the molar yield of condensation reaction is about 70%, and quality difference is big

Method used

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  • Chlorpromazine hydrochloride synthesis process

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Experimental program
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Effect test

Embodiment 1

[0024] The synthesis of embodiment 1 chlorpromazine hydrochloride

[0025] 1. Condensation reaction

[0026] 1) Put 2-chlorophenothiazine and toluene with water into a dry and clean reaction pot, stir and heat, first steam the toluene at normal pressure, and then dry under reduced pressure;

[0027] 2) Add sodium hydroxide, tetrabutylammonium bromide and toluene into the reaction pot in 1) again, stir and heat, reflux for dehydration, and dropwise add N, N-dimethyl-3-chloropropylamine under reflux. Toluene solution, first fast and then slow, drop in about 6 hours, continue to reflux dehydration, until the water output within 30 minutes is less than 10ml, the reaction is considered to be over; wherein 2-chlorophenothiazine and N,N-dimethyl- The mass ratio of 3-chloropropylamine, sodium hydroxide and tetrabutylammonium bromide is 1:0.5:0.9:0.01.

[0028] 3) After the reaction is over, cool the cooling water to below 50°C, add water slowly to prevent flushing, stir, and let it ...

Embodiment 2

[0038] The synthesis of embodiment 2 chlorpromazine hydrochloride

[0039] 1. Condensation reaction

[0040] 1) Put 2-chlorophenothiazine and toluene with water into a dry and clean reaction pot, stir and heat, first steam the toluene at normal pressure, and then dry under reduced pressure;

[0041] 2) Add sodium hydroxide, tetrabutylammonium bromide and toluene into the reaction pot in 1) again, stir and heat, reflux for dehydration, and dropwise add N, N-dimethyl-3-chloropropylamine under reflux. Toluene solution, first fast and then slow, drop in about 6 hours, continue to reflux dehydration, until the water output within 30 minutes is less than 10ml, the reaction is considered to be over; wherein 2-chlorophenothiazine and N,N-dimethyl- The mass ratio of 3-chloropropylamine, sodium hydroxide and tetrabutylammonium bromide is 1:0.7:1.2:0.03.

[0042] 3) After the reaction is over, cool the cooling water to below 50°C, add water slowly to prevent flushing, stir, and let it ...

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Abstract

The invention relates to a chlorpromazine hydrochloride synthesis process, which includes the steps: leading 2-chlorophenothiazine of a primary ring and a side chain of N, N-dimethyl-3-chloropropylamine, which serve as raw materials, to react with sodium hydroxide and tetrabutylammonium bromide, which serve as condensing agent, to generate chlorpromazine; and salifying the chlorpromazine and hydrogen chloride so that chlorpromazine hydrochloride is synthesized. By means of selecting the sodium hydroxide and the tetrabutylammonium bromide as the condensing agent, and strictly controlling the raw material ratio and an indicator end point of salifying reaction, molar yield of the chlorpromazine can be higher than 90%, and the quality of the chlorpromazine hydrochloride meets the requirements of the BP (British Pharmacopoeia).

Description

technical field [0001] The invention relates to a synthesis process of chlorpromazine hydrochloride. Background technique [0002] The representative drug of phenothiazines is a central dopamine receptor blocker with various pharmacological activities, such as treating psychosis, antiemetic, intractable hiccups, hypothermic anesthesia, artificial hibernation, and heart failure. The commonly used synthetic technique of chlorpromazine hydrochloride is to take the 2-chlorophenothiazine of main ring and side chain N, N-dimethyl-3-chloropropylamine as raw material, take sodium hydroxide as condensation agent to react to generate chlorpromazine, Gained chlorpromazine and hydrogen chloride gas are salified, promptly get chlorpromazine hydrochloride, and reaction equation is as follows: [0003] [0004] . The yield of chlorpromazine hydrochloride obtained by the above synthesis process is not very high, and the molar yield of the condensation reaction is about 70%, and the qua...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D279/28
Inventor 王苏南汤金春
Owner 常州康普药业有限公司
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