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Preparation process of phenylhydrazine hydrochloride

A technology of phenylhydrazine hydrochloride and preparation process, which is applied in the preparation of hydrazine, organic chemistry and other directions, can solve the problems of long reaction time and high production cost, and achieve the effects of low production cost, shortened reaction time and high product purity

Inactive Publication Date: 2012-03-21
袁雪冲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Phenylhydrazine hydrochloride is an important intermediate, especially a pharmaceutical intermediate. The prior art uses phenylhydrazine hydrochloride as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare phenylhydrazine salt The synthesis process of acid salt, the reaction time is long, the general required yield is only 63-72%, and the production cost is high

Method used

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Examples

Experimental program
Comparison scheme
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Embodiment Construction

[0009] The specific embodiment of the present invention is described below:

[0010] Add 100ml of water and 57.5ml of 10N hydrochloric acid into a 600ml beaker, stir, add 34.6g of phenylhydrazine hydrochloride, heat to 40°C to dissolve it, then slowly cool the solution to 0°C, and slowly add sodium nitrite solution (made up of 15 grams of sodium nitrite and 30,1 l of water), after adding, adjust the pH of the system to be 1-2, control the temperature of the reaction system at 7°C, react after 30 minutes, stop the reaction, filter and retain the filtrate.

[0011] Add 125ml of water into a 1000ml beaker, add 64 grams of sodium metabisulfite and 65 grams of sodium hydroxide under stirring. At this time, the pH of the solution is 7, and the temperature of the solution is 35°C. After the solution is cooled to 20°C, slowly add the above filtrate, Control the solution temperature to 20°C, pH to 7, continue to reflect for 30 minutes, heat the reaction system to 80°C, stir, add 115ml ...

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Abstract

The invention relates to a preparation process of phenylhydrazine hydrochloride. The preparation process comprises the following steps of: undergoing a diazo reaction and a reduction reaction on phenylhydrazine hydrochloride serving as a starting raw material; and hydrolyzing to prepare phenylhydrazine hydrochloride, wherein the reduction reaction is undergone under the conditions that the temperature is 10-35 DEG C and the pH is 7-9 by taking sodium pyrosulfite as a reducing agent. The phenylhydrazine hydrochloride product prepared with the preparation process has high product purity and low production cost.

Description

technical field [0001] The invention relates to a preparation process of phenylhydrazine hydrochloride. Background technique [0002] Phenylhydrazine hydrochloride is an important intermediate, especially a pharmaceutical intermediate. The prior art uses phenylhydrazine hydrochloride as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare phenylhydrazine salt The synthetic technique of salt, the reaction time is long, the general required yield is only 63-72%, and the production cost is high. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation process for phenylhydrazine hydrochloride, the phenylhydrazine hydrochloride product obtained by the process has high purity and low production cost. [0004] In order to solve the above technical problems, the present invention adopts the following technical solutions: [0005] The preparation process of phenylhy...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/22C07C241/02
Inventor 袁雪冲
Owner 袁雪冲