阅读说明：本技术 一种丁酮肟的合成方法 (Synthesis method of butanone oxime ) 是由 王存亮 许灵艳 严学文 黄焕军 王小桥 于 2018-06-27 设计创作，主要内容包括：本发明公开了一种丁酮肟的合成方法,丁酮中滴加盐酸羟胺乙醇溶液,搅拌升温至50-60℃,肟化反应时间为1-2h,冷却过滤,滤液升温蒸馏,收取152-154℃的馏分,即为丁酮肟；本发明合成条件简单,操作方便,污染小,产率高,耗时短。(The invention discloses a synthetic method of butanone oxime, wherein a hydroxylamine hydrochloride ethanol solution is dripped into butanone, the temperature is raised to 50-60 ℃ by stirring, the oximation reaction time is 1-2h, the cooling and the filtration are carried out, the temperature of the filtrate is raised for distillation, and the fraction with the temperature of 152-154 ℃ is collected, namely the butanone oxime; the method has the advantages of simple synthesis conditions, convenient operation, little pollution, high yield and short time consumption.)

1. A synthetic method of butanone oxime is characterized in that: dripping hydroxylamine hydrochloride ethanol solution into butanone, stirring and heating to 50-60 ℃, carrying out oximation reaction for 1-2h, cooling and filtering, heating and distilling the filtrate, and collecting 152-154 ℃ fraction, namely the butanone oxime.

2. The method for synthesizing butanone oxime according to claim 1, wherein the method comprises the following steps: the weight ratio of the butanone to the hydroxylamine hydrochloride ethanol is 1: 0.9-0.95.

Technical Field

The invention belongs to the field of compound synthesis, and particularly relates to a synthetic method of butanone oxime.

Background

The prior butanone oxime synthesis method comprises the following steps: 2-nitrobutane catalytic hydrogenation, electrochemical methods, oxime exchange methods and the like, and the methods have the disadvantages of large pollution, low yield and long time consumption.

Disclosure of Invention

The invention aims to solve the problems in the existing butanone oxime synthesis method and provide the butanone oxime synthesis method which is convenient to operate, low in pollution, high in yield and short in time consumption.

The invention is realized by the following technical scheme: dripping hydroxylamine hydrochloride ethanol solution into butanone, stirring and heating to 50-60 ℃, carrying out oximation reaction for 1-2h, cooling and filtering, heating and distilling the filtrate, and collecting 152-154 ℃ fraction, namely the butanone oxime.

The weight ratio of butanone to hydroxylamine hydrochloride ethanol in the invention is 1: 0.9-0.95.

The method has the advantages of simple synthesis conditions, convenient operation, little pollution, high yield and short time consumption.

Detailed Description

In this example, 50g butanone is added into a 250mL flask, 95g50% hydroxylamine hydrochloride ethanol solution is dropped into a constant pressure dropping funnel, the temperature is raised to 58 ℃ by stirring, the temperature is kept for 90min, cooling and filtering are performed, the temperature of the filtrate is raised for distillation, and the fraction with the temperature of 152-154 ℃ is collected, namely the butanone oxime.