Method for synthesizing L-menthy chloroformate

A technology for the synthesis of menthyl chloroformate, which is applied in the preparation of phosgene or haloformate, organic chemistry, etc., can solve the problems of high transportation requirements, and achieve the effects of easy reaction measurement, cost reduction, and low production equipment requirements

Inactive Publication Date: 2005-05-18
上海香料研究所
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  • Summary
  • Abstract
  • Description
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Problems solved by technology

At present, phosgene is usually used to react with L-menthol to synthesize L-menthyl chloroformate in China. Phosgene has high requirements for transportation, storage, and production equipment, and has safety and environmental problems.

Method used

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  • Method for synthesizing L-menthy chloroformate

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Embodiment Construction

[0007] Further illustrate the implementation of the present invention below:

[0008] Add 312 grams (2mol) of menthol, 596 grams (2mol) of triphosgene, and 2300ml of dichloromethane in a 5000ml round-bottomed three-necked flask equipped with a stirrer, thermometer, dropping funnel and tail gas absorption device. 606 g (6 mol) of triethylamine was added dropwise at room temperature, and the addition was completed in about 1.5 hours, followed by stirring at room temperature for 10 hours. After the reaction, wash with 1200ml of water, 1200 grams of 5% dilute hydrochloric acid, 200 grams of 5% sodium carbonate, and 800 grams of water, reclaim the solvent, and distill under reduced pressure to obtain 406.5 grams of product, with a content of 98% and a theoretical yield of 93.2%. .

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Abstract

The present invention discloses a kind of L-menthyl chloroformate synthesizing process. Under room temperature and in the presence of catalyst, L-menthol and triphosgene are chloroacylated to obtain L-menthyl chloroformate. The process has reaction temperature of 25 deg.c, reaction time of 10-12 hr and catalyst pyridine, triethylamine or hexahydropyridine. The present invention has the advantages of substituting phosgene with less toxic solid triphosgene, easy control of the reaction, and relatively high safety and environment friendship.

Description

Technical field: [0001] The present invention relates to a kind of synthetic method of L-menthyl chloroformate Background technique: [0002] L-menthyl chloroformate is a raw material for synthesizing L-menthol ethylene glycol carbonate and L-menthol propylene glycol carbonate. Under the condition of room temperature and a catalyst, L-menthyl chloroformate is obtained through acyl chloride reaction with L-menthol and triphosgene. At present, phosgene and L-menthol are usually used in China to react to synthesize L-menthyl chloroformate. Phosgene has relatively high requirements for transportation, storage, and production equipment, and has safety and environmental protection problems. Invention content: [0003] The present invention aims at the shortcomings of the prior art, and the present invention provides a synthetic method for preparing L-menthyl chloroformate that is convenient for transportation, storage, requires low production equipment, and has no safety and en...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/02C07C69/96
Inventor 章平毅
Owner 上海香料研究所
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