A kind of preparation method of ethyl 5-methyl-5-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: 2022-05-24
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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  • A kind of preparation method of ethyl 5-methyl-5-hexenoate
  • A kind of preparation method of ethyl 5-methyl-5-hexenoate

Examples

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Embodiment 1

[0022]In a 500ml clean, dry four-mouth flask, add ethyl acrylate 50g, benzene 200g, with a thermometer, add 4.0g catalyst, catalyst comprising 1.4g aluminum chloride and 2.6g tungsten hexachloride, control temperature 25 °C, through the cylinder gas isobutene 50g, throughisobutene 8h, 25 °C insulation for 24h, and then add (20g sodium bicarbonate and water 100g) of the solution, stirring 0.5h, and then adding (20g 30% hydrochloric acid and water 60g) of the mixture, Stirring 0.5 hours, stationary 0.5 hours, delamination, divided into the lower aqueous layer, washed with 200g of water, layered to obtain the aqueous layer and benzene layer; benzene layer into the barrel, add 1g of dehydrating agent dehydration overnight, dehydrating agent including 0.5g of anhydrous sodium sulfate and 0.5g of n-butanol, concentrated to 50L volume, first atmospheric pressure and then reduced pressure, and then put into the distillation kettle, kettle temperature 95 ° C , top temperature of 75 ° C, ja...

Embodiment 2

[0024] In a 500ml clean, dry four-mouth flask, add ethyl acrylate 50g, benzene 220g, with a thermometer, add 5.0g catalyst, catalyst comprising 1.8g aluminum trichloride and 3.2g tungsten hexachloride, control temperature 28 ° C, through the cylinder gas isobutylene 60g, through about 12h, 28 ° C insulation for 48h, and then add (20g sodium bicarbonate and water 100g) solution, stirring 0.5h, and then adding (20g 30% hydrochloric acid and water 80g) of the mixture, Stir 0.5h, stationary 0.5h, layer, remove the lower aqueous layer, wash with 200g of water to get the aqueous layer and the benzene layer; put the benzene layer into the bucket, add 1g of dehydrating agent to dehydrate overnight, the dehydrating agent comprises 0.6gwt% Anhydrous sodium sulfate and 0.4g n-butanol are concentrated to 55L volume, first atmospheric pressure and then decompression, and then put into the distillation kettle for rectification, the kettle temperature is 100 °C, the top temperature is about 75 °...

Embodiment 3

[0026]In a 500ml clean, dry four-mouth flask, add ethyl acrylate 50g, benzene 250g, with a thermometer, add 6.0g catalyst, catalyst comprising 2.4g aluminum chloride and 3.6g tungsten hexachloride, control temperature 30 °C, through the cylinder gas isobutylene 65g, through about 16h, 30 °C insulation for 60 hours, and then add (20g sodium bicarbonate and water 100g) solution, stirring for 0.5 hours, and then adding (20g 30% hydrochloric acid and water 100g) of the mixture, Stirring 0.5h, stationary 0.5h, layering, divided into the lower aqueous layer, washed with 200g of water, layered to obtain the aqueous layer and benzene layer; benzene layer into the barrel, add dehydrating agent dehydration overnight, dehydrating agent including 0.7g anhydrous sodium sulfate and 0.3g n-butanol, concentrated to 60L volume, first atmospheric pressure and then decompression, and then put into the distillation kettle, kettle temperature 120 ° C, top temperature of about 75 ° C, jacket about 70 °...

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Abstract

The invention discloses a preparation method of ethyl 5-methyl-5-hexenoate, comprising the following steps: 1) adding ethyl acrylate, benzene and a catalyst into a four-necked flask, controlling the temperature to 25-30° C. Add isobutylene, keep the temperature for 24-60h, add aqueous sodium bicarbonate solution, stir for 0.5-1h, then add a mixture of hydrochloric acid and water, stir for 0.5h, stand still for 0.5h, separate layers, and wash with water to obtain an aqueous layer and a benzene layer; 2 ) adding the benzene layer into the barrel, adding a dehydrating agent for dehydration, concentrating, first at normal pressure, then under reduced pressure, rectifying, and collecting the normal boiling fraction to obtain 5-methyl-5-ethyl hexenoate. The invention provides a preparation method of ethyl 5-methyl-5-hexenoate, using aluminum trichloride and tungsten hexachloride synergistically as a catalyst, and the total yield can reach more than 46.7%. When butanol is used as a dehydrating agent, the product purity can reach more than 97.5%; the preparation method of the invention is simple in operation and low in cost.

Description

Technical field [0001] The present invention relates to a method for preparing ethyl 5-methyl-5-hexenoate. Background [0002] In the prior art, the addition reaction between ethyl acrylate and isobutene in the presence of a catalyst is a commonly used method for preparing ethyl 5-methyl-5-hexenoate, the method yield is low, only about 20%, resulting in higher product costs. Contents of the Invention [0003] In response to the problems of the above prior art, the present invention provides a method for preparing ethyl 5-methyl-5-hexenoate. [0004] To solve the above technical problems, the technical solution employed in the present invention is: [0005] A method for preparing ethyl 5-methyl-5-hexenoate, wherein the preparation method comprises the following steps: [0006] 1) Ethyl acrylate, benzene and catalyst are added to the four-mouth flask, the temperature is controlled 25-30 ° C, through the isobutene, 25 ~ 30 ° C insulation for 24 ~ 60 h, and then add the aqueous sodi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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