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Menthyl lactate preparation method

A technology of menthyl lactate and lactic acid, applied in the field of high-yield preparation of novel cooling agent menthyl lactate, can solve the problems of trivial details and high equipment requirements, and achieve the effect of improving the yield

Inactive Publication Date: 2014-12-17
HENAN ACADEMY OF SCI CHEM RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method is relatively cumbersome, and the raw materials must be distilled under reduced pressure first, and the equipment requirements are relatively high.

Method used

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  • Menthyl lactate preparation method

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Experimental program
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Effect test

Embodiment 1

[0017] Add 15.6 g of menthol, 23.5 g of 90% lactic acid, 0.1 g of sulfuric acid, and 50 g of toluene into a 250 ml three-neck flask equipped with a thermometer and a water separator, and heat to reflux for 2.5 hours. Cool down to 10°C, pour directly into 200g saturated calcium sulfate solution, stir for 6 hours, filter, separate layers, dry the oil layer with toluene, filter, and distill under reduced pressure to obtain 21.8g of the product, detected by gas chromatography, the content of menthyl lactate is 93.58 %, menthol is 5.54%, and lactoyl ester of menthyl lactate is 0.12%. The yield of menthyl lactate was 89.5% based on menthol added and 97.0% based on menthol reacted.

Embodiment 2

[0019] Add 15.6 g of menthol, 25 g of 90% lactic acid, 0.2 g of sulfuric acid, and 60 g of toluene into a 250 ml three-neck flask equipped with a thermometer and a water separator, and heat to reflux for 3 hours. Cool down to 20°C, pour 200g of Na with a pH of 9.0 directly 2 HPO 4 -NaH 2 PO 4 In the buffer solution, stir for 6 hours, filter, separate layers, filter the oil layer after drying with magnesium sulfate, and distill under reduced pressure to obtain 22.3g of the product. Gas chromatography detection shows that the content of menthyl lactate is 94.5%, and menthol is 4.34%. The lactoyl ester of the ester is 0.09%. The yield of menthyl lactate was 92.4% based on menthol added and 99.0% based on menthol reacted.

Embodiment 3

[0021] Add 15.6 g of menthol, 23.5 g of 90% lactic acid, 0.2 g of sulfuric acid, and 60 g of toluene into a 250 ml three-neck flask equipped with a thermometer and a water separator, and heat to reflux for 4 hours. Cool down to 5°C, add 150g of Na with a pH of 8.0 directly 2 HPO 4 -NaH 2 PO 4 Buffer solution, stirred for 6 hours, filtered, separated, the oil layer was dried with magnesium sulfate, filtered, and distilled under reduced pressure to obtain 22.5g of the product, detected by gas chromatography, the content of menthyl lactate was 93.6%, and menthol was 4.82%. Menthyl lactate The lactoyl esters are 0.11%. The yield of menthyl lactate was 92.3% based on menthol added and 95.3% based on menthol reacted.

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Abstract

The invention discloses a menthyl lactate preparation method with high yield, and belongs to the field of organic chemical synthesis production. The method comprises the following steps of: taking excessive lactic acid and menthol as raw materials, directly generating menthyl lactate and lactoylic esters including menthyl lactyl lactate, menthyl lactoyl lactyl lactate under an effect of a catalyst. The menthyl lactate and the lactoylic esters without any other treatments are directly added into a buffer solution or an acidic salt saturated solution for stirring for several hours, the pH value of the reaction solution is not needed to control, and the conversion from the high-level lactoylic esters to the menthyl lactate is realized, so that the generation of the menthyl lactate with high yield is realized. The menthyl lactate preparation method is simple in generating technology, high in yield, liable to obtain raw materials, and free from specific reaction, separation and purification equipments.

Description

technical field [0001] The invention relates to a high-yield preparation method of a novel cooling agent menthyl lactate, which belongs to the field of organic chemical synthesis. Background technique [0002] Menthyl Lactate is a high-efficiency, new type of cooling agent with long-lasting, mild, cool and fresh mint flavor, considered as a substitute for menthol, widely used in various products using mint flavor flavor, such as toothpaste It can also be used in candy, beverages, and as a mint flavor enhancer in oral care products. In 2006, menthyl lactate was identified from Indian mint oil, which allowed manufacturers to declare it a natural or natural-equivalent product, depending on how it was prepared. In April 2012, China released the national standard for menthyl lactate (GB 28338-2012 National Food Safety Standard Food Additive L-Menthyl Lactate). [0003] Using lactic acid and menthol as raw materials to directly react menthyl lactate to prepare a large number of ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C69/68C07C67/08C07C67/60
Inventor 代本才赵永德陈瑨霍萃萌王兰天张豫黎
Owner HENAN ACADEMY OF SCI CHEM RES INST CO LTD