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Method for synthesizing 2,4-dimethyl phenylhydrazine hydrochloride

A technology of dimethylphenylhydrazine and a synthesis method is applied in the synthesis process conditions of phenylhydrazine hydrochloride and the synthesis technology field of pharmaceutical intermediates, and can solve the problems of easy introduction of impurities, low yield, etc.

Inactive Publication Date: 2011-05-25
TIANJIN POLYTECHNIC UNIV
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Problems solved by technology

There are many ways to synthesize phenylhydrazine hydrochloride derivatives. The most commonly used method is to use the corresponding aniline derivatives as raw materials and realize them through diazotization, addition reduction, acid precipitation and other processes. This route is easy to introduce impurities and the yield is low. High disadvantage

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  • Method for synthesizing 2,4-dimethyl phenylhydrazine hydrochloride

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Embodiment Construction

[0010] The present invention will be further described below in conjunction with specific examples.

[0011] Literature reference example:

[0012] Synthetic Chemistry 2006, 14(3): 317-318 Example:

[0013] Dissolve 28.1g (50mmol) in 6mL glacial acetic acid in a beaker, heat to 70°C, quickly pour into hydrochloric acid [20mL (150mmol)] preheated to 30°C, stir for 25min, and quickly cool to 0°C with an ice-salt bath . Add sodium nitrite aqueous solution (3.6g sodium nitrite dissolved in 6.7mL water) dropwise within 6 minutes, add crushed ice at the same time to control the reaction temperature below 5°C, and react for 45 minutes to obtain the reaction solution A containing 3.

[0014] Dissolve 13 g of sodium bisulfite in 40 mL of water in a three-necked flask, adjust the pH to 6 with 40% aqueous sodium hydroxide solution, and cool to 5°C. The reaction solution A (below 10°C) was added dropwise within 20 minutes. At the same time, 40% sodium hydroxide solution was added dro...

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Abstract

The invention discloses a method for synthesizing 2,4-dimethyl phenylhydrazine hydrochloride, which is characterized in that the material adding proportion of raw materials of 2,4-dimethylaniline to sodium nitrite to sodium sulfite is 1 / 1.05 / 2.5, the zinc powder consumption is 0.05 times of the 2,4-dimethylaniline consumption; the diazo reaction is carried out at the temperature between 0 DEG C and 5 DEG C, the sodium nitrite is added within 10 minutes, and the diazotization is completed within 10 to 15 minutes; the reduction reaction is carried out at 100 DEG C when the pH value is about 6; and the acidulation temperature is 80 DEG C. The reaction is carried out under the process condition, the yield of obtained products is higher than 90 percent, and the purity is higher than 99 percent.

Description

technical field [0001] The invention relates to a synthesis process of a drug intermediate, in particular to a synthesis process condition of phenylhydrazine hydrochloride, and belongs to the field of synthesis of a drug intermediate. Background technique [0002] Phenylhydrazine hydrochloride derivatives are a very important class of chemical raw materials, commonly used in the fields of medicine, dyes, pesticides, and photosensitive materials, such as the synthesis of rimonabant, an analgesic, and the synthesis of analgesic etodolac. Synthesis of White Agent AD, Synthesis of Tinopal WG and Synthesis of Developer Accelerator, etc. In addition, the derivatives of phenylhydrazine hydrochloride can also be used as crystallization agents for the determination of the absolute configuration of chiral ketones. There are many ways to synthesize phenylhydrazine hydrochloride derivatives. The most commonly used method is to use the corresponding aniline derivatives as raw materials ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C243/22C07C241/02
Inventor 刘冬青颜范勇任松
Owner TIANJIN POLYTECHNIC UNIV
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