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Method for preparing mixed dibasic acid mono-L-menthyl acetate by using nylon acid

A technology of mixing dibasic acid and nylon acid, applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as reports on the research of synthetic methods, and achieve significant economic value and high yield , the effect of generating a simple process

Active Publication Date: 2014-05-07
CHINA TOBACCO HENAN IND +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on its synthetic method in China.

Method used

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  • Method for preparing mixed dibasic acid mono-L-menthyl acetate by using nylon acid
  • Method for preparing mixed dibasic acid mono-L-menthyl acetate by using nylon acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Add 75g of nylon acid and 120g of acetic anhydride to a 500ml three-neck flask equipped with a thermometer and a condenser tube and heat to reflux for 6 hours. Distilled under reduced pressure to remove acetic acid and remaining acetic anhydride, added 100 g of extraction solvent toluene, stirred, heated to reflux, cooled and filtered to obtain 11.0 g of crude adipic acid, which was recrystallized from water to obtain 9.0 g of adipic acid with a content of 98.5%. Evaporate part of the solvent from the filtrate under reduced pressure, add 0.9g of catalyst DMAP and 78g of menthol, heat at 100°C for 9 hours, filter, add 200g of 5% sodium carbonate solution by mass percentage, stir and separate layers, add 3N hydrochloric acid to the water layer, and adjust the pH value 3, stirred, extracted with chloroform, dried the organic layer, filtered and distilled off the solvent under pressure, and dried to obtain 132.4 g of mixed dibasic acid mono-L-menthyl ester, with a total cont...

Embodiment 2

[0022] Add 75g of nylon acid and 120g of acetic anhydride to a 500ml three-neck flask equipped with a thermometer and a condenser tube and heat to reflux for 6 hours. Distilled under reduced pressure to remove acetic acid and the remaining acetic anhydride, added 100 g of chloroform as an extraction solvent, stirred, heated to reflux, cooled and filtered to obtain 10.2 g of crude adipic acid, which was recrystallized from water to obtain 8.4 g of adipic acid with a content of 98.6%. Part of the solvent was evaporated from the filtrate under reduced pressure, 0.9 g of catalyst dipotassium hydrogen phosphate and 78 g of menthol were added, heated to reflux for 8 hours, filtered, 200 g of a 5% sodium carbonate solution by mass percentage was added, the layers were stirred, and 3N hydrochloric acid was added to the water layer to adjust The pH value was 1, stirred, extracted with chloroform, dried the organic layer, filtered and distilled off the solvent under pressure, and dried t...

Embodiment 3

[0024] Add 75g of nylon acid and 120g of acetic anhydride to a 500ml three-neck flask equipped with a thermometer and a condenser tube and heat to reflux for 6 hours. Distilled under reduced pressure to remove acetic acid and the remaining acetic anhydride, added 100 g of petroleum ether as an extraction solvent, stirred, heated to reflux, cooled and filtered to obtain 12.0 g of crude adipic acid, which was recrystallized from water to obtain 9.2 g of adipic acid with a content of 98.1%. Evaporate part of the solvent from the filtrate under reduced pressure, add 0.9 g of catalyst sodium sulfate and 78 g of menthol, heat at 120 ° C for 6 hours, filter, add 200 g of 5% by mass sodium carbonate solution, stir and separate layers, add 3N hydrochloric acid to the water layer, and adjust the pH The value was 2, stirred, extracted with chloroform, dried the organic layer, filtered and distilled off the solvent under pressure, and dried to obtain 134.3 g of mixed dibasic acid mono-L-me...

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Abstract

The invention discloses a method for preparing mixed dibasic acid mono-L-menthyl acetate by using nylon acid and belongs to the field of organic chemical synthesis. The method comprises the following steps: by taking the nylon acid as an initial raw material, obtaining a binary anhydride (comprising glutaric anhydride and butanedioic anhydride) mixture through acetic anhydride dehydration; and further reacting with menthol, and obtaining mixed dibasic acid mono-L-menthyl acetate (comprising glutaric acid mono-L-menthyl acetate and butanedioic acid mono-L-menthyl acetate). The production process is simple, the raw materials are easily available, the yield is high, special reaction or separation and purification equipment is not needed, and the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing novel cooling agent mixed dibasic acid mono-L-menthyl (including mono-L-menthyl glutarate and mono-L-menthyl succinate) from nylon acid, which belongs to the field of organic chemical synthesis. Background technique [0002] Nylon acid, also known as mixed dibasic acid, is a mixture of succinic acid, glutaric acid and adipic acid, which is a by-product of the production of adipic acid. In 2013, the domestic production of adipic acid reached 700,000 tons. According to the current production technology level, 50-60kg of nylon acid will be recovered for every ton of adipic acid produced, and 35,000-42,000 tons of nylon acid will be produced in China every year. by-product. [0003] There are many domestic and foreign research reports on the utilization of nylon acid produced in the process of producing adipic acid, including the separation and purification of mixed dibasic acids. So far, the methods develo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/42C07C69/40C07C67/08
CPCC07C67/08C07C2601/14C07D307/60C07D309/32C07C69/42C07C69/40
Inventor 马宇平陈芝飞芦昶彤赵永德陈瑨代本才霍萃萌
Owner CHINA TOBACCO HENAN IND
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