Method for preparing 4-chlorine phenylhydrazine

A kind of technology of chlorophenylhydrazine and chloroaniline, applied in the field of preparation of 4-chlorophenylhydrazine, can solve the problems of high production cost, long reaction time and the like

Inactive Publication Date: 2008-04-09
太仓市华联化工实业有限公司
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  • Abstract
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AI Technical Summary

Problems solved by technology

[0002] 4-chlorophenylhydrazine is an important intermediate, especially a pharmaceutical intermediate. The prior art uses 4-chloroaniline as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare 4-chlorophenylhydrazine The synthetic method of hydrazine, reaction time is long, generally needs yield to be only 63-72%, and production cost is high

Method used

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Examples

Experimental program
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Embodiment Construction

[0008] The specific embodiment of the present invention is described below:

[0009] Add 100ml of water to an 800ml beaker, stir, add 57.5ml of 10N hydrochloric acid, 25.7 grams of 4-chloroaniline, after all dissolve, cool the solution to 0°C, slowly add sodium nitrite solution (from 15 grams of sodium nitrite and 30ml water), after adding, adjust the pH of the system to 1-2, control the temperature of the reaction system to 3-5° C., stop the reaction after 20 minutes of reaction, filter and retain the filtrate.

[0010] Add 250ml 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 10°C, slowly add the above filtrate, When the addition is complete, the solution temperature is 16°C, pH is 7, continue to react for 30 minutes, heat the reaction system to 75-80°C, stir, add 115ml of hydrochloric aci...

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Abstract

The invention relates to a preparative method of 4-chlorophenyl hydrazi. By using 4-chloraniline as the initial raw material, the preparative method is capable of producing the 4-bromophenylhydrazine after the diazotization reaction, the reduction reaction and hydrolysis, wherein, the reduction reaction which utilizes sodium metabisulfite as the reduction agent is carried out under the conditions that the temperature is 10 to 35 DEG C and the PH is 7 to 9. The 4- chlorophenyl hydrazi produced by the preparative method of the invention is characterized in high product purity and low production cost.

Description

technical field [0001] The invention relates to a preparation method of 4-chlorophenylhydrazine. Background technique [0002] 4-chlorophenylhydrazine is an important intermediate, especially a pharmaceutical intermediate. The prior art uses 4-chloroaniline as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare 4-chlorophenylhydrazine The synthetic method of hydrazine has a long reaction time, generally requires a yield of 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 method of 4-chlorophenylhydrazine, the 4-chlorophenylhydrazine product obtained by the method 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] A preparation method of 4-chlorophenylhydrazine, using 4-chloroaniline as ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/22C07C241/02
Inventor 沈云汉郁金龙
Owner 太仓市华联化工实业有限公司
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