Preparation method of paracyano-group phenyl hydrazine hydrochloride

A technology of cyanophenylhydrazine and hydrochloride, which is applied in the field of preparation of aromatic hydrazine hydrochloride synthesis, can solve problems such as low yield and poor crystal form, achieve short production time, low requirements for production equipment, The effect of high overall yield
CN101550091AInactive Publication Date: 2009-10-07上海药明康德新药开发有限公司
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
上海药明康德新药开发有限公司
Publication Date
2009-10-07
Estimated Expiration
Not applicable · inactive patent

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Abstract

The invention relates to a preparation method for compounding fragrant hydrazine, in particular to a preparation method of paracyano-group phenyl hydrazine hydrochloride, which mainly solves the technical problems of poor crystal shape and low yield of the prior preparation method. The adopted technical scheme is as follows: the preparation method of the paracyano-group phenyl hydrazine hydrochloride is characterized in that: paracyano-group aniline is used as a raw material and is prepared into diazo hydrochloride in a hydrochloric water solution by the diazotizing reaction of sodium nitrite in the mode of one-step continuous reacting operation, the diazo hydrochloride is reduced by a tin-protochloride hydrochloric solution, filtered and washed to obtain paracyano-group phenyl hydrazine hydrochloride, and the paracyano-group phenyl hydrazine hydrochloride is recrystallized by the mixed solution of methanol and water to obtain a white crystal target product. The paracyano-group phenyl hydrazine hydrochloride obtained by the invention is an important normal medical intermediate product.
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Description

Technical field:

[0001] The invention particularly relates to a preparation method for the synthesis of aromatic hydrazine hydrochloride, in particular to a preparation method for p-cyanophenylhydrazine hydrochloride. Background technique:

[0002] P-cyanophenylhydrazine is a relatively important commonly used drug intermediate. For the preparation of p-cyanophenylhydrazine, the literature reports also use p-cyanoaniline as a raw material, which is obtained by reacting with sodium nitrite and tin dichloride / concentrated hydrochloric acid successively. p-Cyanophenylhydrazine as the hydrochloride salt. But what obtain is white powder, and yield is only 70%. Therefore, find a kind of suitable solvent to carry out recrystallization, obtain good crystal form, improve product yield and just become the key problem that the present invention needs to solve. Invention content:

[0003] The purpose of the present invention is to provide a synthetic method for effectively preparing...

Claims

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