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Synthesis method for organic synthesis of intermediate acetyl phenylhydrazine

A technique for the synthesis of acetylbenzene and its synthesis method, which is applied in the field of synthesis of the organic synthesis intermediate acetylphenylhydrazine, which can solve the problems of complex process and low final yield, reduce intermediate links, shorten reaction time, and improve reaction Yield effect

Inactive Publication Date: 2018-07-06
CHENGDU DONG DIAN AI ER TECH
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  • Claims
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Problems solved by technology

But, existing synthetic method mostly adopts acid anhydride as reactant, and process is more complicated, and final yield is not very high, therefore, be necessary to propose a kind of new synthetic method, this is for further improving the quality of product and yield, reduces By-product content is economically important

Method used

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  • Synthesis method for organic synthesis of intermediate acetyl phenylhydrazine

Examples

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Effect test

example 1

[0011] Add 3mol phenylhydrazine and 4mol p-iodoacetanilide to the reaction vessel, heat to 90°C, reflux for 130min, lower the temperature to 10°C, filter the crystals, wash with 80% methylamine solution and 85% dichloromethane The solution was washed, recrystallized in 90% ethanol solution, the crystals were precipitated, filtered, and dehydrated with anhydrous magnesium sulfate dehydrating agent to obtain 391.5 g of the finished product, acetylphenylhydrazine, with a yield of 87%.

example 2

[0013] Add 3mol phenylhydrazine and 4.5mol p-iodoacetanilide to the reaction vessel, heat to 92°C, reflux for 140min, lower the temperature to 12°C, filter the crystals, wash with 83% methylamine solution and 87% dichloro Wash with methane solution, recrystallize in 93% ethanol solution, precipitate crystals, filter, and dehydrate with activated alumina dehydrating agent to obtain 409.5 g of the finished product, acetylphenylhydrazine, with a yield of 91%.

example 3

[0015] Add 3mol phenylhydrazine and 5mol p-iodoacetanilide to the reaction vessel, heat to 95°C, reflux for 150min, lower the temperature to 15°C, filter the crystals, wash with 86% methylamine solution and 90% dichloromethane solution Wash, recrystallize in 96% ethanol solution, precipitate crystals, filter, and dehydrate with anhydrous magnesium sulfate dehydrating agent to obtain 418.5 g of the finished product, acetylphenylhydrazine, with a yield of 93%.

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Abstract

The invention relates to a synthesis method for organic synthesis of an intermediate acetyl phenylhydrazine. The method mainly includes the steps of: adding 3mol phenylhydrazine into a reaction container and 4-5mol p-iodoacetanilide into a reaction container, performing heating to 90-95DEG C, conducting reflux for 130-150min, lowering temperature to 10-15DEG C, filtering the crystal, conducting washing with a methylamine solution and a dichloromethane solution respectively, performing recrystallization in an ethanol solution, precipitating crystals, conducting filtration, and performing dehydration with a dehydrating agent, thus obtaining the finished product acetyl phenylhydrazine.

Description

technical field [0001] The invention relates to a method for synthesizing an organic synthesis intermediate, acetylphenylhydrazine. Background technique [0002] Acetyl phenylhydrazine is mainly used in organic synthesis and stabilizer. But, existing synthetic method mostly adopts acid anhydride as reactant, and process is more complicated, and final yield is not very high, therefore, be necessary to propose a kind of new synthetic method, this is for further improving the quality of product and yield, reduces The by-product content is of great economic importance. Contents of the invention [0003] The object of the present invention is to provide a kind of synthetic method of organic synthesis intermediate acetylphenylhydrazine, comprising the steps: [0004] (i) Add 3mol phenylhydrazine and 4-5mol p-iodoacetanilide to the reaction vessel, heat to 90-95°C, reflux for 130-150min, lower the temperature to 10-15°C, filter the crystals, wash with methylamine solution, Was...

Claims

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Application Information

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IPC IPC(8): C07C243/28C07C241/04
CPCC07C241/04C07C243/28
Inventor 严义达
Owner CHENGDU DONG DIAN AI ER TECH
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