Method for preparing 2-hydrazinobenzoic acid hydrochloride

A technology of hydrochloride and carboxybenzene, applied in the field of preparation of 2-carboxyphenylhydrazine hydrochloride, can solve the problems of difficult transportation and storage, many equipment and high cost, and achieves shortened reduction reaction time, high product purity, and high production efficiency. low cost effect

Inactive Publication Date: 2009-01-07
太仓市华联化工实业有限公司
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

The synthetic method of this traditional phenylhydrazine hydrochloride, the reaction time is as long as 3~4 hours, and the yield is only between 63-72%. In addition, when the reducing agent used is sodium sulfite and sodium bisulfite, the cost Higher, increase production cost; and when ammonium bisulfite and ammonium hydroxide are used as reducing agents, because they are liquid, it is not easy to transport and store
In addition, reduction kettle, pressure filter and acid analysis kettle are used in this process, which requires a lot of equipment and large investment.

Method used

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Examples

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Embodiment Construction

[0016] A specific embodiment of the present invention will be described below, but it is not limited to this example.

[0017] According to the preparation method of the 2-carboxyphenylhydrazine hydrochloride of the present embodiment, comprises the steps:

[0018] (1), diazotization reaction

[0019] Add 200ml of water and 27.4g of 2-aminobenzoic acid to an 800ml beaker, stir, add 57.5g of 10N hydrochloric acid, and stir thoroughly for 30 minutes. After the 2-aminobenzoic acid is completely dissolved, slowly cool the solution to below 0°C, and then slowly Add sodium nitrite aqueous solution (formed by dissolving 15g sodium nitrite and 30ml water), after adding, the material temperature in the beaker is 5°C, and it is slightly blue to potassium iodide iodine powder test paper. Control the temperature of the material at 0-5° C., continue to stir and react for 20 minutes, and filter to obtain 400-450 ml of a brown solution, which is the benzenediazonium chloride solution.

[0...

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PUM

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Abstract

The invention relates to a method for preparing 2-carboxyl phenyl hydrazine, which comprises the following steps: (1) 2-aminobenzoic acid is used as starting material, and benzene diazonium chloride is prepared through diazo reaction; (2) benzene diazonium chloride obtained from the step (1) is utilized to further prepare reduction products through the reduction reaction under the action of a reducing agent; (3) the reduction products obtained from the step (2) undergoes the hydrolysis reaction under the action of hydrochloric acid to generate 2-carboxyl phenyl hydrazine, more particularly, sodium metabisulfite is used as the reducing agent in the reduction reaction in the step (2), and the reaction is performed under the condition that the temperature is 15 to 25 DEG C and the pH value is 7 to 9. The method has higher yield, and can shorten the production period and reduce the manufacture cost at the same time.

Description

technical field [0001] The invention relates to a preparation method of phenylhydrazine hydrochloride, in particular to a preparation method of 2-carboxyphenylhydrazine hydrochloride. Background technique [0002] 2-Carboxylphenylhydrazine hydrochloride is an important intermediate, which is mainly used to prepare indole and pyrazolone derivatives, and can also be used to prepare other chemical products. The traditional preparation process of 2-carboxyphenylhydrazine hydrochloride includes a two-step process of diazotization of aniline and reduction of benzenediazonium chloride, wherein the diazotization of aniline is mostly in hydrochloric acid medium, under the condition of pH equal to 2, at 0~ Add sodium nitrite to react at a low temperature of 5°C to generate benzenediazonium chloride. Sodium sulfite and sodium bisulfite are generally used as reducing agents for the reduction of diazobenzene chloride, and ammonium bisulfite and ammonium hydroxide are also used as reduci...

Claims

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Application Information

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