Preparation method of chlorphenesin carbamate

A technology of chlorphenesin carbamate and chlorphenesin, which is applied in the field of preparation of chlorphenesin carbamate

Inactive Publication Date: 2010-01-13
朱岩安
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, there is no domestic product listed in the domestic market for medicines prepared using chlorphenglycerolbamate as a raw material medicine. The present in

Method used

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Examples

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Embodiment

[0013] Add 161.1 grams of chlorphenesin and 135 grams of diethyl carbonate to a clean and dry reaction flask equipped with electric stirring, a thermometer, and a condenser, heat to 40°C to 50°C, add 3.0 grams of sodium ethylate, and continue heating Transesterification reaction, after reacting for 1.5 hours, distill under reduced pressure to remove the organic solvent, lower the temperature slightly, add 2 ml of dimethylformamide, 98 ml of tert-butanol, and then add 300 ml of 25% industrial ammonia water. Ammonification reaction at 0°C for 9 hours, refrigerated at about 0°C for 4 hours, then filtered with suction, crushed the filter cake, soaked in ammonia water containing 1% ammonia at 0°C to 5°C for 1 hour, filtered with suction, and dried to obtain crude chlorophenylglycerin Urethane, then refined with the mixed solvent that 120 milliliters of ethanol and 60 milliliters of ethyl acetate that have 2 milliliters of 25% analytical pure ammonia water added form 118 grams of ela...

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PUM

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Abstract

The invention relates to a preparation method of chlorphenesin carbamate, which comprises the following steps: heating chlorphenesin and reacting the chlorphenesin with diethyl carbonate under the action of less ester exchange catalyst; adding tertiary butanol and dimethyl formamide to be used as mixed solvent after the reaction is finished, reacting the mixture with ammonia water to prepare a target object, filtering, and washing by using pure water containing less ammonia; and refining by using ethanol containing less ammonia and ethyl acetate as mixed solvent to obtain the chlorphenesin carbamate of raw material medicine. The used solvents have lower toxicity and hazard, the refining method is special and comprises the steps of washing by the pure water containing less ammonia to remove most of impurities and refining by taking ethanol with less ammonia and the ethyl acetate as the mixture, thereby leading the product not to nearly contain toxic and hazardous organic solvent and optimizing the production environment.

Description

technical field [0001] The invention relates to a preparation method of chlorophenglycerolamine. Background technique [0002] The present invention refers to chlorophenylglycerol carbamate, molecular formula is C 10 h 12 ClNO 4 , the English name is Clorphenesin Carbamate or (RS)-3-(4-chlorophenoxy)-2-hydroxypropylcarbamate; the chemical name is chlorphenesin carbamate or (±)-3-(4-chlorophenoxy)- 1,2-Propanediol-1-urea. [0003] In order to prolong the time of action of the representative drug of central muscle relaxants and to reduce its toxic and side effects, Upjohn Company of the United States conducted a series of substitution studies on the groups of the benzene ring of the central muscle relaxants and the Discuss their efficacy and persistence and other related issues. From 1957 to the second year, they changed the ortho methoxy group on the Shujinling molecule to a para halogen group. As a result, it was found that the drug has a longer duration of action than...

Claims

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Application Information

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IPC IPC(8): C07C271/12C07C269/00C07C269/08
Inventor 朱岩安
Owner 朱岩安
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