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Preparation method of 2-amino-5-chlorobenzophenone oxime

A technology of benzophenone oxime and chlorobenzophenone is applied in the directions of oxime preparation, organic chemistry, etc., can solve the problems of easy punching, cumbersome post-processing operation, low total reaction yield and the like, and achieves short reaction time, The reaction process is easy to control, and the reaction process has no side effects.

Inactive Publication Date: 2021-03-30
BEIJING YIMIN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The post-treatment operation of this preparation method is loaded down with trivial details, is easy to punch material, and the total yield of reaction is low, therefore, research the preparation method of 2-amino-5 chloro-benzophenone oxime, improve synthesis process, improve the conversion rate of reaction, improve quality and Yield and cost reduction are of great significance

Method used

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  • Preparation method of 2-amino-5-chlorobenzophenone oxime

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Effect test

Embodiment 1

[0032] A preparation method of 2-amino-5 chloro-benzophenone oxime, comprising the following steps

[0033] (1) Selection of raw materials: select ethanol 3450ml, 2-amino-5-chlorobenzophenone 490g, hydroxylamine hydrochloride 185g, NaOH 200g, quantitative acetic acid and water;

[0034] (2) Reaction: Put 3450ml of ethanol into a 5L reaction bottle, start stirring, then put in 490g of 2-amino-5-chlorobenzophenone, 185g of hydroxylamine hydrochloride and 200g of NaOH, put the bottle cap on, seal the feeding port, and heat up After treatment, add activated carbon and reflux for 3 hours to obtain the reactant 2-amino-5-chloro-benzophenone oxime. The molar ratio of sodium oxide is 1.0:2.0, and the volume ratio of aminoketone weight to ethanol is 1.0:5.0;

[0035] (3) Distillation: After step (2), add 1kg of water to the reaction bottle, continue heating to distill out ethanol, when the ethanol is no longer distilled, add 2kg of water to the reaction bottle, stir for 25min, at this...

Embodiment 2

[0041] A preparation method of 2-amino-5 chloro-benzophenone oxime, comprising the following steps

[0042] (1) Selection of raw materials: select ethanol 3550ml, 2-amino-5-chlorobenzophenone 510g, hydroxylamine hydrochloride 190g, NaOH 205g, quantitative acetic acid and water;

[0043] (2) Reaction: Put 3550ml of ethanol into a 5L reaction bottle, start stirring, then put in 510g of 2-amino-5-chlorobenzophenone, 190g of hydroxylamine hydrochloride and 205g of NaOH, put the bottle cap on, seal the feeding port, and heat up After treatment, add activated carbon and reflux for 3 hours to obtain the reactant 2-amino-5 chloro-benzophenone oxime. The molar ratio of sodium oxide is 1.0:2.2, and the volume ratio of aminoketone weight to ethanol is 1.0:6.0;

[0044] (3) Distillation: After step (2), add 1kg of water to the reaction bottle, continue heating to distill out ethanol, when the ethanol is no longer distilled, add 2kg of water to the reaction bottle, stir for 35min, at this...

Embodiment 3

[0050] A preparation method of 2-amino-5 chloro-benzophenone oxime, comprising the following steps

[0051](1) Selection of raw materials: select ethanol 3600ml, 2-amino-5-chlorobenzophenone 515g, hydroxylamine hydrochloride 200g, NaOH 215g, quantitative acetic acid and water;

[0052] (2) Reaction: Put 3600ml of ethanol into a 5L reaction bottle, start stirring, then put in 515g of 2-amino-5-chlorobenzophenone, 200g of hydroxylamine hydrochloride and 215g of NaOH, put the bottle cap on, seal the feeding port, and heat up After treatment, add activated carbon to reflux for 3 hours to obtain the reactant aminoketone, the temperature of the reaction system is 70°C, the molar ratio of aminoketone to hydroxylamine hydrochloride is 1.0:1.5, the molar ratio of aminoketone to sodium hydroxide is 1.0:2.8, The volume ratio of aminoketone weight to ethanol is 1.0:8.0;

[0053] (3) Distillation: After step (2), add 1kg of water to the reaction bottle, continue heating to distill ethanol...

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Abstract

The invention relates to the field of pharmaceutical chemicals, in particular to a preparation method of 2-amino-5-chlorobenzophenone oxime. The invention aims to solve the problems of complicated post-treatment operation, easiness in material flushing, low total reaction yield, low quality and high cost of conventional preparation methods. According to a scheme in the invention, the preparation method comprises the following steps: (1) selection of raw materials: selecting 3400-3600 ml of ethanol, 480-520 g of 2-amino-5-chlorobenzophenone, 180-210 g of hydroxylamine hydrochloride, 200-225 g of NaOH, quantitative acetic acid and quantitative water; and (2) reaction: adding ethanol into a reaction bottle with a volume of 5 L, and starting stirring. The preparation method is simple and convenient in process, short in reaction time, mild in reaction conditions, easy to control in reaction process and free of side reactions, a reaction conversion rate is increased, product yield is high, and the prepared product is high in purity; product separation and purification treatment are convenient and rapid, so a final product with relatively high purity can be obtained; and the reaction product is easy to purify, the reaction process has no pollution to the environment, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to the field of medicine and chemical industry, in particular to a preparation method of 2-amino-5-chloro-benzophenone oxime. Background technique [0002] 2-Amino-5-chloro-benzophenone oxime is an important starting material or intermediate for the preparation of oxazepam, its CAS number: 18097-52-4, and its structural formula is: ,Wide range of applications. [0003] At present, the commonly used preparation method of 2-amino-5-chloro-benzophenone oxime is: use 2-amino-5-chloro-benzophenone to react with hydroxylamine hydrochloride, and obtain 2-amino -5-Chlorobenzophenone reactant, after adding liquid alkali to adjust the pH to 8, add activated carbon to reflux for 30min, filter while hot, add hydroxylamine hydrochloride to the filtrate and reflux for 10h, recover ethanol (75%), add water to dilute to ethanol concentration of 4-5%, cool to 30°C, add saturated sodium carbonate solution to pH 9, filter, wash the filter cake wi...

Claims

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Application Information

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IPC IPC(8): C07C249/08C07C249/14C07C251/48
CPCC07C249/08C07C249/14
Inventor 史鸿聪赵海涛何立涛彭金金黄玉华李丽丙崔健
Owner BEIJING YIMIN PHARMA
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