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Method for preparing n-amyl cinnamate by transesterification reaction catalyzed by ionic liquid

A technology of n-amyl cinnamate and exchange reaction is applied in the field of chemical industry and achieves the effects of good stability, easy post-processing and low energy consumption

Inactive Publication Date: 2012-07-25
GUANGDONG IND TECHN COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no systematic research on the use of microwave control and ionic liquid catalysts in the transesterification reaction process

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 1.6219g (0.01mol) methyl cinnamate and 0.2595g 1-butyl-3-methylimidazole p-toluenesulfonate in the microwave reaction tank of WF-4000 atmospheric pressure microwave rapid reaction system (the same below), and then Add 0.1 mol of n-amyl alcohol and mix thoroughly to obtain the reaction raw material; microwave the reaction raw material for 45 minutes, set the microwave power to 200W, and set the microwave irradiation temperature to 137°C, and obtain a colorless product after microwave irradiation. Using gas-mass spectrometry to carry out qualitative and quantitative analysis on the obtained product, the conversion rate of methyl cinnamate is calculated to be 27.43%.

[0032] The resulting product was assayed as follows:

[0033] 1. Determination of physical constants: The product was purified and then measured for its refractive index. The refractive index was 1.5384 (30°C), which was consistent with the measured value of the standard product; the boiling point was: 2...

Embodiment 2

[0037] Add 1.6219g (0.01mol) methyl cinnamate and 0.2595g 1-butyl-3-methylimidazole p-toluenesulfonate into a microwave reaction tank, then add 0.1mol n-amyl alcohol, and mix well to obtain the reaction raw material ; The reaction raw materials were irradiated with microwaves for 30 minutes, the microwave power was set to 400 W, and the microwave irradiation temperature was set to 137° C. After microwave irradiation, a light yellow product was obtained. Qualitative and quantitative analysis was carried out on the obtained product by gas-mass spectrometry, and the conversion rate of methyl cinnamate was calculated to be 29.45%.

[0038] The resulting product was assayed as follows:

[0039] 1. Determination of physical constants: The product was purified and then measured for its refractive index. The refractive index was 1.5384 (30°C), which was consistent with the measured value of the standard product; the boiling point was 205-207°C (2000Pa), which was consistent with the l...

Embodiment 3

[0043] Add 1.6219g (that is, 0.01mol) methyl cinnamate and 0.2271g 1-butyl-3-methylimidazole p-toluenesulfonate into a microwave reaction tank, then add 0.08mol n-pentanol, and mix well to obtain the reaction Raw materials: Microwave irradiation was carried out on the reaction raw materials for 30 minutes, the microwave power was set to 400 W, and the microwave irradiation temperature was set to 110° C., and a light yellow product was obtained after microwave irradiation. Qualitative and quantitative analysis was carried out on the obtained product by gas-mass spectrometry, and the conversion rate of methyl cinnamate was calculated to be 19.72%.

[0044] The resulting product was assayed as follows:

[0045] 1. Determination of physical constants: The product was purified and then measured for its refractive index. The refractive index was 1.5384 (30°C), which was consistent with the measured value of the standard product; the boiling point was 205-207°C (2000Pa), which was co...

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Abstract

The invention belongs to the technical field of chemistry and chemical engineering, and discloses a method for preparing n-amyl cinnamate by a transesterification reaction catalyzed by ionic liquid. The method comprises the following steps of: mixing methyl cinnamate, 1-butyl-3-methylimidazole p-toluenesulfonate 14-16% of the weight of methyl cinnamate, and n-amyl alcohol evenly, performing radiation with 100-500W microwave for 5-60 min at a set temperature of 90-137 DEG C, and carrying out separation to obtain n-amyl cinnamate, wherein the conversion rate of methyl cinnamate reaches 29.45%. The method provided by the invention adopts a novel technique of a microwave assisted transesterification reaction catalyzed by 1-butyl-3-methylimidazole p-toluenesulfonate ionic liquid to synthesize n-amyl cinnamate, and the method has the advantages of high heating efficiency, greatly shortened reaction time, low energy consumption, high efficiency, simple process, easiness in post treatment, recyclable catalyst, environmental friendliness and the like. The method is consistent with the concept of sustainable development, is an environment-friendly energy-saving green chemical method, and has a good industrialization prospect.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and relates to a method for preparing n-pentyl cinnamate by catalyzing transesterification with ionic liquid, in particular to a method for catalyzing 1-butyl-3-methylimidazole p-toluenesulfonate ionic liquid in cooperation with microwave The invention discloses a method for preparing n-pentyl cinnamate through the transesterification reaction between methyl cinnamate and n-pentanol. Background technique [0002] Cinnamate is an important class of synthetic fragrances, which are widely used in ingredients of food flavors and daily chemical flavors because of their special fruity or floral fragrance, and are also important raw materials for organic synthesis. N-pentyl cinnamate is a balsamic ester with cocoa aroma, which is widely used in the preparation of edible and daily chemical flavors in industry. [0003] At present, the synthesis method of cinnamate is mainly th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/618C07C67/03
CPCY02P20/584
Inventor 黎彧
Owner GUANGDONG IND TECHN COLLEGE
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