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Method for synthesizing L-menthol glycol carbonic ester

A technology of menthol ethylene glycol carbonate and ethanol carbonate, which is applied in the field of synthesis of L-menthol ethylene glycol carbonate, can solve the problem of high requirements and low yield of L-menthol ethylene glycol carbonate, High cost and other issues, to achieve the effect of high product yield

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

The synthesis method currently adopted uses phosgene or substances capable of producing phosgene in the reaction process. Phosgene has high requirements for transportation, storage, and production equipment, and the cost is high, and what is obtained is L-mint with a low yield. Brain Glycol Carbonate

Method used

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  • Method for synthesizing L-menthol glycol carbonic ester

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Embodiment Construction

[0007] Further illustrate the implementation of the present invention below: the preparation of L-menthol alcohol carbonate: add the chloroform of 250ml in the 1000ml round bottom three-necked flask that agitator, dropping funnel, inner thermometer are housed, 108.5 grams (1mol) chloroformic acid Ethyl ester, 78 g (0.5 mol) menthol, start stirring, add 55.5 g (0.5 mol) triethylamine dropwise at room temperature, the dropwise addition is completed in about 1 hour, and then keep warm at 60°C for 8-10 hours. Stop stirring, wash with dilute hydrochloric acid and water respectively, then recover the solvent, and then distill under reduced pressure to obtain 103 grams of product, the content is 98%, and the theoretical yield is 90%.

[0008] The preparation of L-menthol ethylene glycol carbonate: add 62 grams (1mol) ethylene glycol, 229 grams (1mol) L-menthol Brain alcohol carbonate, 10 grams of MCM-41-TBD, start stirring, and react at about 125°C for 15 hours. Stirring was stopped...

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PUM

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Abstract

The present invention discloses a kind of L-menthol glycol carbonic ester synthesizing process. In the first step, menthol and ethyl chloroformate are reacted at 60 deg.c for 9-11 hr in the presence of catalyst pyridine or triethylamine to prepare to prepare L-menthol ethanol carbonic ester. In the second step, L-menthol ethanol carbonic ester and glycol produce alcohol exchange reaction of 10-15 hr to obtain L-menthol glycol carbonic ester at 125 deg.c and in the presence of catalyst MCM-41-TBD or HIGH-TDB. The present invention has the advantages of no use and production of phosgene and the catalyst MCM-41-TBD or HIGH-TDB used in the second step with high catalytic activity and capable of being reused.

Description

Technical field: [0001] The invention relates to a synthesis method of L-menthol ethylene glycol carbonate applied to food and daily chemical products. Background technique: [0002] L-menthol ethylene glycol carbonate is a natural equivalent, which is characterized by a suitable cooling effect on the skin or human mucous membranes, and is suitable for food and daily chemical products. The synthesis method currently adopted uses phosgene or substances capable of producing phosgene in the reaction process. Phosgene has high requirements for transportation, storage, and production equipment, and the cost is high, and what is obtained is L-mint with a low yield. Brain Glycol Carbonate. Invention content: [0003] Aiming at the shortcomings of the prior art, the invention provides an improved synthesis method of L-menthol ethylene glycol carbonate, and obtains low-cost, high-yield L-menthol ethylene glycol carbonate. [0004] The synthetic method of L-menthol ethylene glycol...

Claims

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Application Information

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IPC IPC(8): C07C68/00C07C69/96
Inventor 章平毅
Owner 上海香料研究所
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