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A kind of synthetic method of Menthyl Methyl Glycol

A kind of technology of methyl ethylene glycol ester and synthetic method, applied in the synthesis field of menthyl methyl glycol ester, can solve problems such as low reaction yield, many by-products, inability to carry out, and achieve high selectivity, high reaction efficiency and the like. Mild conditions, simple purification effect

Active Publication Date: 2022-04-22
KUNSHAN YAXIANG SPICEL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method is prone to coupling reactions, resulting in more by-products and lower yields
Another kind of process is to utilize menthyl formic acid to be prepared into sodium salt, and then obtain ethylene glycol menthyl carbonate with chloroethanol under the catalysis of pyridine. There are following problems in this method: cyclization reaction occurs in chloroethanol under the action of pyridine, so that the reaction The yield is extremely low, and it is even impossible to carry out

Method used

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  • A kind of synthetic method of Menthyl Methyl Glycol
  • A kind of synthetic method of Menthyl Methyl Glycol

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Dissolve 35g (0.19mol) of menthyl formic acid and 13g (0.21mol) of ethylene glycol with 100ml of toluene and put them into the reaction flask, adjust the temperature in the reaction flask to 0-10°C; put 30g of pyridine (0.38mol) into the reaction , Dissolve 40g (0.21mol) of p-toluenesulfonyl chloride in 100ml of toluene, then put it into the dropping funnel and drop it slowly. After the reaction is completed, the reaction mixture is first adjusted to PH=1 to 3 with 5 to 10% hydrochloric acid, stirred for 1 hour, and then the mixture is adjusted to PH to 12 to 14 with 10% aqueous sodium hydroxide solution, extracted with toluene , Distilled to obtain menthol methyl glycol ester 36g with a content of 97% and a yield of 84%.

Embodiment 2

[0019] Dissolve 500g (2.72mol) of menthyl formic acid and 170g (2.73mol) of ethylene glycol with 1L of toluene and put them into a reaction flask, adjust the temperature in the reaction flask to 0-10°C; put 430g of pyridine (5.44mol) into the reaction , Dissolve 515g (2.73mol) of p-toluenesulfonyl chloride in 1.5L toluene, then put it into the dropping funnel and slowly drop it in. 8 hours, after the reaction was finished, the reaction mixture was first adjusted to PH=1 to 3 with 5 to 10% hydrochloric acid, stirred for 1 hour, then the mixture was adjusted to PH=12 to 14 with 10% aqueous sodium hydroxide solution, Extraction and distillation yielded 545.7 g of menthyl methyl glycol ester with a content of 98% and a yield of 88%.

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Abstract

The invention discloses a method for synthesizing menthyl methyl glycol ester. Drop into pyridine in the reaction, then drop into p-toluenesulfonyl chloride solution, after the dripping is completed, after the reaction finishes, the treatment reaction obtains Menthyl Methyl Glycol; A kind of Menthyl Methyl Glycol of the present invention Synthesis of esters by using the better leaving group TsO ‑ , the reaction conditions are mild, the yield is as high as more than 80%, and because the p-methylbenzenesulfo group is large, the self-epoxidation reaction and cross-linking reaction of ethylene glycol are blocked, the selectivity is high, and the synthesis process is one-step synthesis , the purification is simple, and the technological process is convenient to operate.

Description

technical field [0001] The invention relates to the field of cooling agent synthesis, in particular to a method for synthesizing menthyl methyl glycol ester. Background technique [0002] Menthol methyl glycol ester, also known as ethylene glycol menthyl carbonate, is a cooling agent that can be used in cosmetics and food. It can not only be widely used as a cooling agent, but also an important Chemical intermediates. [0003] Existing synthetic ethylene glycol menthyl carbonate, a kind of process is to utilize menthyl formic acid to make acid chloride, then react with ethylene glycol to obtain the product. This method is prone to coupling reactions, resulting in more by-products and lower yields. Another kind of process is to utilize menthyl formic acid to be prepared into sodium salt, and then obtain ethylene glycol menthyl carbonate with chloroethanol under the catalysis of pyridine. There are following problems in this method: cyclization reaction occurs in chloroethan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/75C07C67/08
CPCC07C67/08C07C69/75
Inventor 周军学陈清
Owner KUNSHAN YAXIANG SPICEL CO LTD