Chlorphenesin carbamate and preparation method thereof

A technology of chlorphenesin carbamate and chlorphenesin ether, which is applied in the preparation of carbamic acid derivatives, chemical instruments and methods, and the preparation of organic compounds, can solve the problems of low production safety and achieve improved production safety, Simplified production process and low cost

Inactive Publication Date: 2010-10-06
ZHEJIANG JIUXU PHARMA +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Therefore, the production safety o

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  • Chlorphenesin carbamate and preparation method thereof
  • Chlorphenesin carbamate and preparation method thereof
  • Chlorphenesin carbamate and preparation method thereof

Examples

Experimental program
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Example Embodiment

Example 1

In a 500ml dry and clean reaction flask equipped with a reflux device, a stirring device and a thermometer, add 202.6g (1mol) of dried chlorophenylglycerol, 200g (1.69mol) of diethyl carbonate, and sodium monooxide on alumina (JAM-6 type) 4g, then put the reaction flask into the microwave reactor, set the microwave radiation power to 100W, and irradiate for 150 minutes.

Take out the reaction flask from the microwave reactor, add 100ml of water to the reaction flask under the condition that the reaction product ethanol exists in the reaction flask, cool to 30~20℃, add 60g (1.1mol) ammonium chloride and sodium hydroxide 44g (1.1mol), then cooled to 15-5°C, stirred for 5h and then cooled to 0°C, stopped stirring, and precipitated crystals. Then use a Buchner funnel to filter, and the resulting filter cake (solid matter remaining on the Buchner funnel) is washed three times with 500 ml of pure water, the filter cake is filtered to dry the water, and then recrystallized w...

Example Embodiment

Example 2

In a 500ml dry and clean reaction flask equipped with a reflux device, a stirring device and a thermometer, add 202.6g (1mol) of dried chlorophenylglycerol, 200g (1.69mol) of diethyl carbonate, and sodium monooxide on alumina (JAM-6 type) 4g, then put the reaction flask into the microwave reactor, set the microwave radiation power to 100W, and irradiate for 150 minutes.

Take out the reaction flask from the microwave reactor, add 100ml of water to the reaction flask under the condition that the reaction product ethanol exists in the reaction flask, cool to 30~20℃, add 100g ammonium carbonate (1.04mol) and 44g sodium hydroxide (1.1mol), then cool to 15-5°C, stir for 5h and then cool to 0°C, stop stirring, and precipitate crystals. Then it was filtered using a Buchner funnel, the filter cake was washed three times with 500 ml of pure water, the filter cake was filtered to dry the water and then recrystallized with butanol twice the weight of the filter cake to obtain 20...

Example Embodiment

Example 3

In a 500ml dry and clean reaction flask equipped with a reflux device, a stirring device and a thermometer, add 202.6g (1mol) of dried chlorophenylglycerol, 200g (1.69mol) of diethyl carbonate, and sodium monooxide on alumina (JAM-6 type) 4g, then put the reaction flask into the microwave reactor, set the microwave radiation power to 100W, and irradiate for 150 minutes.

Take out the reaction flask from the microwave reactor, add 100ml of water to the reaction flask under the condition that the reaction product ethanol exists in the reaction flask, cool to 30~20℃, add 60g ammonium chloride (1.1mol) and 59g sodium methoxide (1.1mol), then cool to 15-5°C, stir for 5h and then cool to 0°C, stop stirring, and precipitate crystals. Then it was filtered using a Buchner funnel, the filter cake was washed three times with 500 ml of pure water, the filter cake was filtered to dry the water and then recrystallized with butanol twice the weight of the filter cake to obtain 201.9...

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Abstract

The invention discloses chlorphenesin carbamate and a preparation method thereof. The preparation method comprises the step of mixing a compound shown in a formula (1) with ammonium reagent and alkali in an organic solvent in the presence of water at the temperature of 0-40 DEG C. The preparation method in the invention utilizes a raw material containing ammonium ions so as to avoid using of strong pungent ammonia water, improves production safety and is favor of environment protection.

Description

technical field The present invention relates to chlorophenyl glyceryl carbamate and preparation method thereof. Background technique Chlorphenesin Carbamate, as a muscle relaxant, has high curative effect and few side effects. At present, the synthesis route of chlorphenesin carbamate is mainly to react chlorphenesin ether with diethyl carbonate to generate a cyclic ether, which is further reacted with ammonia water to prepare chlorphenesin carbamate. Chinese patent application CN10162435 discloses a preparation method of chlorphenesin urethane, specifically, chlorphenesin reacts with diethyl carbonate under the action of a small amount of transesterification catalyst, and then adds tert-butanol, dimethylformamide and ammonia water, Chlorphenglyceryl carbamate. Owing to use ammoniacal liquor in above-mentioned synthetic route, and ammoniacal liquor is volatile, has strong irritant, has irritant to respiratory tract and skin, and damages central nervous system. If ammon...

Claims

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Application Information

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IPC IPC(8): C07C271/12C07C269/00
Inventor 潘自国李宏于自勋岳昌林陈美兰
Owner ZHEJIANG JIUXU PHARMA
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