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Synthesis method of 3-methyl-2-butene-1-geranoil formate

A technology of alcohol formate and synthesis method, which is applied in the preparation of carboxylate, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low synthesis rate and long synthesis period, and achieves improved yield and accelerated reaction. Effect of time, high product yield

Active Publication Date: 2018-06-08
GUANGXI FORESTRY RES INST
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For this reason, the technical problem to be solved by this invention is to provide a kind of synthetic method of 3-methyl-2-butene-1-alcohol formate, to solve 3-methyl-2-butene- The synthesis period of 1-alcohol formate is longer and the synthesis rate is slightly lower

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Embodiment 1 ionic liquid preparation

[0018] The ionic liquid required by the following embodiments of the present invention is N, N, N', N'-tetramethyl-N"-octylguanidine trifluoromethyl acetate ionic liquid ([HOctTMG]CF 3 COO), its synthetic method comprises the steps:

[0019] (1) Dissolve 0.30mol of tetramethylurea in 175mL of toluene, and drop into freshly steamed 0.31mol of POCl under nitrogen protection and stirring conditions 3 After reacting at room temperature for 10 hours, 0.70 mol of n-octylamine was added dropwise. After completion, it was stirred at room temperature for 34 hours. After diluting the reaction system with 175 mL of water, it was vigorously stirred for 30 minutes. The lower layer solution was taken, and solid NaOH was added thereto until The system shows alkalinity, then the solution is divided into two layers, and the solid is filtered off. After the filtrate is separated, take the upper layer solution, dissolve it in ether, and then use an...

Embodiment 2

[0022] In a 250mL three-necked flask equipped with a thermometer, a reflux condenser, and a dropping funnel, add 86g of 3-methyl-2-buten-1-ol and 60g of formic acid (molar ratio 1:1.3), and then add sodium bisulfite 0.43g (0.5wt%) was used as a catalyst, and then the three-neck flask was placed in a heating mantle with magnetic stirring to heat the reaction (35° C.) and the magnetic stirring was turned on to carry out the esterification reaction for 6 hours. After the reaction is over, the reaction product is washed to neutrality, and the product is detected according to the prior art method (see "Technology Research on the Synthesis of α-Bisabolol from Dipentene", Deng Qian, etc.), and the product 3- The yield of methyl-2-buten-1-ol formate was 94.3%.

Embodiment 3

[0024] In a 250mL three-neck flask equipped with a thermometer, a reflux condenser, and a dropping funnel, add 86g of 3-methyl-2-buten-1-ol and 64.4g of formic acid (molar ratio 1:1.4), and then add hydrogen sulfite Sodium 0.86g (1wt%) was used as a catalyst, and then the three-neck flask was placed in a heating mantle with magnetic stirring to heat the reaction (35° C.) and the magnetic stirring was turned on to carry out the esterification reaction for 5 hours. After the reaction is over, the reaction product is washed to neutrality, and the product is detected according to the prior art method (see "Technology Research on the Synthesis of α-Bisabolol from Dipentene", Deng Qian, etc.), and the product 3- The yield of methyl-2-buten-1-ol formate was 94%.

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Abstract

The invention belongs to the technical field of chemical synthesis and particularly relates to a synthesis method of 3-methyl-2-butene-1-geranoil formate. According to the synthesis method of the 3-methyl-2-butene-1-geranoil formate and on the basis of the existing technical process, sodium hydrogen sulfite serves as a catalyst, the yield of a 3-methyl-2-butene-1-geranoil formate product is further increased, more preferably, reaction is conducted under the existence of ionic liquid, the reaction time is effectively increased besides the yield of the products is effectively increased, and higher product yield can be obtained within shorter time.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a synthesis method of 3-methyl-2-buten-1-ol formate. Background technique [0002] Bisabolol, also known as sweet bisabolol and fangfeng root alcohol, is one of the most abundant sesquiterpene compounds in nature. Bisabolol has two structures of α-body and β-body. α-Bisabolol mainly exists in chamomile essential oil, gum poplar essential oil and some essential oils of the genus Placifera and Salvia; β- Bisabolol mainly exists in cotton bud essential oil, corn oil, camphor oil and frankincense oil. Bisabolol has good stability and skin compatibility, and is suitable for use in cosmetics; at the same time, bisabolol has medicinal effects such as anti-inflammatory, sterilizing, healing ulcers, and dissolving gallstones. It has a wide range of uses in the pharmaceutical industry; in addition, because bisabolol has a light and pleasant aroma, it is also a stab...

Claims

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Application Information

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IPC IPC(8): C07C67/08C07C69/06
CPCC07C67/08C07C69/06Y02P20/54
Inventor 秦荣秀李桂珍梁忠云陈海燕周丽珠谷瑶
Owner GUANGXI FORESTRY RES INST
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