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Synthesis method of diphenyl ketone hydrazone

A technology for the synthesis of benzophenone hydrazone, which is applied in the preparation of hydrazone, organic chemistry, etc., can solve the problems of unsafety, long reaction time, and low yield, and achieve the effects of increasing yield, process safety, and improving yield

Inactive Publication Date: 2013-10-09
RUGAO ZHONGCHANG CHEM
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Problems solved by technology

Wherein, benzophenone oxime and diphenyldiazomethane are expensive, and there are few manufacturers, so they have not been widely used; at present, in the synthetic method of taking benzophenone as raw material, anhydrous hydrazine and Benzophenone is refluxed in absolute ethanol to make benzophenone hydrazone, and anhydrous hydrazine is a kind of highly dangerous chemicals that are very easy to spontaneously ignite and explode, and it is extremely unsafe. Defects such as low rate

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  • Synthesis method of diphenyl ketone hydrazone
  • Synthesis method of diphenyl ketone hydrazone
  • Synthesis method of diphenyl ketone hydrazone

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Embodiment 1

[0019] After confirming that the equipment is all in good condition and that there is no foreign matter in the reactor, 500 kg of dehydrated alcohol is first vacuumed into the reactor, 100 kg of benzophenone is added, and then 40 kg of hydrazine hydrate and 8 kg of hydrochloric acid are drawn in.

[0020] After all the raw materials are put in, turn on the steam to raise the temperature. When the temperature of the material in the reactor reaches 95°C, start to bring water. The reaction solution was cooled to 10°C for crystallization, stirred for 1 hour, and then started to filter. During the filter, it was necessary to ensure that the filtrate was dried to ensure that there was no n-butanol dripping out of the outlet of the centrifuge. The filter time was 35 minutes.

[0021] After shaking, put the solid product into the reaction kettle, add 400 kg of pure water and about 400ml of glacial acetic acid for soaking, add the dried solid and stir for 2 hours, and start to filter af...

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Abstract

The invention discloses a synthesis method of diphenyl ketone hydrazone, which comprises the following steps: sucking anhydrous ethanol into a reaction kettle via vacuum; then, adding diphenyl ketone, hydrazine hydrate and hydrochloric acid, and performing hydrazone generation reaction; when the temperature in the reaction kettle reaches 90-100 DEG C, cooling the reaction solution with cooling water while stirring, thus precipitating crystals; performing centrifugal filtration, then adding the solid product into the reaction kettle, adding pure water and glacial acetic acid, and soaking; and stirring, performing centrifugal filtration to ensure that the filtrate is dried through centrifugal filtration, and drying under reduced pressure to obtain the finished product. According to the method, the hydrochloric acid is used as a catalyst instead, so that the output is improved and the yield is obviously increased on the premise of ensuring the quality; and anhydrous hydrazine is very prone to spontaneous combustion and spontaneous explosion, and the 80-85% hydrazine hydrate is used instead, thereby ensuring safe process and better effect.

Description

technical field [0001] The invention relates to a synthesis method of a compound, in particular to a synthesis method of benzophenone hydrazone. Background technique [0002] Benzophenone hydrazone is an important organic chemical raw material, which is widely used in the fields of photosensitive materials, spices, ultraviolet absorbers, organic pigments, medicines and insecticides. Benzophenone hydrazone can be used to produce palazoxacin, dicyclohexyl piperidine, diphenhydramine hydrochloride and antiarrhythmic drug cibenzoline succinate, etc., and can also be used as antibiotic drugs (such as cefixime, cefrazone and β-lactamase inhibitor tazobactam, etc.) in the synthesis process of 6-APA and 7-ACA carboxyl protecting group; benzophenone hydrazone can be used to prepare diphenyldiazomethane (DPM) and its related compounds , dimethyldiazomethane is widely used for carboxyl protection in the synthesis of penicillins and cephalosporins; benzophenone hydrazone is the main r...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C251/86C07C249/16
Inventor 王朝阳
Owner RUGAO ZHONGCHANG CHEM
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