Preparation method for 4-sulfonamidophenylhydrazine hydrochloride

A technology of sulfonylaminophenylhydrazine and sulfonylaminoaniline, which is applied in the preparation of sulfonamides, organic chemistry, etc., can solve the problems of long reaction time and high production cost, and achieve low production cost, shortened reaction time and high product purity Effect

Inactive Publication Date: 2008-03-26
太仓市华联化工实业有限公司
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Problems solved by technology

[0002] P-sulfonylaminophenylhydrazine is an important intermediate, especially a pharmaceutical intermediate. The prior art uses p-sulfonylaminoaniline as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare p-sulfonylaminophenylhydrazine The synthetic method of amide phenylhydrazine, reaction time is long, and generally required yield is only 63-72%, and production cost is high

Method used

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Embodiment Construction

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

[0009] Add 3.44 grams of p-sulfonylaminoaniline, 10 ml of water, and 5 ml of 10N hydrochloric acid into a 100 ml flask, stir and dissolve, and after cooling to below 0° C., add sodium nitrite solution (made up of 1.38 grams of sodium nitrite and 2.76 ml of water), React at 0-5°C for 5 minutes, filter to remove residue, and obtain diazonium salt solution.

[0010] Sodium pyrosulfite 6.4g, water 25ml, 10N sodium hydroxide 5ml, stirring and dissolving to make sodium pyrosulfite alkaline solution, after cooling to 10-20°C, add the above diazonium salt solution, adjust the pH to 7-8, at 20-30 After reacting at ℃ for 30 minutes, add 10ml of 10N hydrochloric acid, heat to 90-103℃, after reacting for 30 minutes, add 0.1 g of activated carbon, filter to remove slag, cool to 10℃, filter, purify, and dry to obtain the product. The instrument detects that its purity is 99.5%.

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Abstract

The present invention relates to preparation process of p-sulfonylamino phenyl hydrazine. The compound p-sulfonylamino phenyl hydrazine is prepared with p-sulfonylamino aniline as initial material, and through diazo reaction, reduction reaction and hydrolysis. The reduction reaction has sodium pyrosulfite as the reductant and the reaction conditions of 10-35 deg.c temperature and pH 7-9. The p-sulfonylamino phenyl hydrazine preparing process has high product purity and low production cost.

Description

technical field [0001] The invention relates to a preparation method of p-sulfonamidophenylhydrazine. Background technique [0002] P-sulfonylaminophenylhydrazine is an important intermediate, especially a pharmaceutical intermediate. The prior art uses p-sulfonylaminoaniline as a raw material, undergoes diazotization reaction, sodium sulfite reduction, and hydrolysis to prepare p-sulfonylaminophenylhydrazine The synthesis method of amidophenylhydrazine has a long reaction time, generally requires a yield of only 63-72%, and high production cost. Contents of the invention [0003] The technical problem to be solved by the present invention is to provide a preparation method of p-sulfonylaminophenylhydrazine, the p-sulfonylaminophenylhydrazine 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 for p-sul...

Claims

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Application Information

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IPC IPC(8): C07C311/38C07C303/40
Inventor 沈云汉
Owner 太仓市华联化工实业有限公司
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