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Preparation method of 5-methyl-5-ethyl hexenoate

A technology of ethyl hexenoate and ethyl acrylate, which is applied in the field of preparation of ethyl 5-methyl-5-hexenoate, can solve the problems of high cost and low yield, achieve low cost, simple operation, The effect of mild reaction conditions

Active Publication Date: 2020-12-11
太仓市茜泾化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] In the prior art, the addition reaction of ethyl acrylate and isobutylene in the presence of a catalyst is a commonly used method for preparing ethyl 5-methyl-5-hexenoate. The yield of this method is low and can only reach 20%. around, resulting in higher product costs

Method used

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  • Preparation method of 5-methyl-5-ethyl hexenoate
  • Preparation method of 5-methyl-5-ethyl hexenoate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 500ml clean and dry four-neck flask, add 50g of ethyl acrylate and 200g of benzene, equipped with a temperature measuring tube, add 4.0g of catalyst, the catalyst includes 1.4g of aluminum trichloride and 2.6g of tungsten hexachloride, and control the temperature at 25°C. Pass 50g of isobutene into the steel cylinder, pass through isobutene for 8h, keep warm at 25°C for 24h, then add a solution of (20g of sodium bicarbonate and 100g of water), stir for 0.5h, then add a mixture of (20g of 30% hydrochloric acid and 60g of water), and stir for 0.5 hour, stand still for 0.5 hour, separate layers, remove the lower water layer, wash with 200g water, separate layers to obtain the water layer and benzene layer; put the benzene layer in a bucket, add 1g dehydrating agent to dehydrate overnight, the dehydrating agent includes 0.5g anhydrous Sodium sulfate and 0.5g n-butanol, concentrated to a volume of 50L, first under normal pressure and then under reduced pressure, then pla...

Embodiment 2

[0024] In a 500ml clean and dry four-neck flask, add 50g of ethyl acrylate and 220g of benzene, equipped with a temperature measuring tube, add 5.0g of catalyst, the catalyst includes 1.8g of aluminum trichloride and 3.2g of tungsten hexachloride, and control the temperature at 28°C. Pass 60g of isobutylene into the steel cylinder for about 12h, keep warm at 28°C for 48h, then add the solution of (20g of sodium bicarbonate and 100g of water), stir for 0.5h, then add the mixture of (20g of 30% hydrochloric acid and 80g of water), and stir 0.5h, stand still for 0.5h, separate layers, remove the lower water layer, wash with 200g water to obtain the water layer and benzene layer; put the benzene layer into a bucket, add 1g dehydrating agent to dehydrate overnight, the dehydrating agent includes 0.6gwt% Sodium sulfate water and 0.4g n-butanol are concentrated to a volume of 55L, first under normal pressure and then under reduced pressure, and then placed in a rectification kettle fo...

Embodiment 3

[0026] In a 500ml clean and dry four-neck flask, add 50g of ethyl acrylate and 250g of benzene, equipped with a temperature measuring tube, add 6.0g of catalyst, the catalyst includes 2.4g of aluminum trichloride and 3.6g of tungsten hexachloride, control the temperature at 30°C, Pass 65g of isobutene into the steel cylinder for about 16h, keep warm at 30°C for 60 hours, then add the solution of (20g of sodium bicarbonate and 100g of water), stir for 0.5 hours, then add the mixture of (20g of 30% hydrochloric acid and 100g of water), Stir for 0.5h, stand still for 0.5h, separate layers, remove the lower water layer, wash with 200g water, separate layers to obtain a water layer and a benzene layer; put the benzene layer in a bucket, add a dehydrating agent to dehydrate overnight, and the dehydrating agent includes 0.7g Sodium sulfate water and 0.3g n-butanol are concentrated to a volume of 60L, first at normal pressure and then under reduced pressure, and then placed in a rectif...

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Abstract

The invention discloses a preparation method of 5-methyl-5-ethyl hexenoate. The method comprises the following steps: 1) adding ethyl acrylate, benzene and a catalyst into a four-neck flask, controlling the temperature to be 25-30 DEG C, introducing isobutene, preserving heat for 24-60 hours, adding a sodium bicarbonate aqueous solution, stirring for 0.5-1 hour, adding a mixed solution of hydrochloric acid and water, stirring for 0.5 hour, standing for 0.5 hour, layering, and washing with water to obtain a water layer and a benzene layer; and 2) adding the benzene layer into a barrel, adding adehydrating agent, dehydrating, concentrating, carrying out normal pressure distillation and reduced pressure distillation in sequence, and collecting the azeotropic fraction to obtain the 5-methyl-5-ethyl hexenoate. According to the preparation method of the 5-methyl-5-ethyl hexenoate, aluminum trichloride and tungsten hexachloride are synergistically used as catalysts, the total yield can reach46.7% or above, anhydrous sodium sulfate and n-butyl alcohol are used as dehydrating agents, and the product purity can reach 97.5% or above; and the preparation method disclosed by the invention issimple to operate and relatively low in cost.

Description

technical field [0001] The invention relates to a preparation method of ethyl 5-methyl-5-hexenoate. Background technique [0002] In the prior art, the addition reaction of ethyl acrylate and isobutylene in the presence of a catalyst is a commonly used method for preparing ethyl 5-methyl-5-hexenoate. The yield of this method is low and can only reach 20%. Left and right, resulting in higher product costs. Contents of the invention [0003] Aiming at the above-mentioned problems in the prior art, the present invention provides a method for preparing ethyl 5-methyl-5-hexenoate. [0004] In order to solve the problems of the technologies described above, the technical solution adopted in the present invention is: [0005] A preparation method of ethyl 5-methyl-5-hexenoate, wherein the preparation method comprises the steps of: [0006] 1) Add ethyl acrylate, benzene and catalyst into a four-necked flask, control the temperature at 25-30°C, pass in isobutylene, keep warm at...

Claims

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Application Information

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IPC IPC(8): C07C67/347C07C69/533B01J27/132
CPCC07C67/347B01J27/132C07C69/533
Inventor 秦正浩吴健明
Owner 太仓市茜泾化工有限公司
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