Method for recycling by-product in preparation process of ethyl 8-halooctanoate

A technology for the preparation process of ethyl octoate, which is applied in the field of recovery and utilization of by-products in the process of ethyl 8-halooctanoate, and can solve the problem that the former fraction cannot be used.

Inactive Publication Date: 2019-08-09
启东东岳药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The by-product can be removed by rectification, but because the boiling points of ethyl 8-ethoxyoctanoate and ethyl 8-halogenated octanoate are close, there will be 8-15% of the front fraction that cannot be utilized

Method used

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  • Method for recycling by-product in preparation process of ethyl 8-halooctanoate
  • Method for recycling by-product in preparation process of ethyl 8-halooctanoate

Examples

Experimental program
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Effect test

Embodiment 1

[0016] In a 500mL three-necked flask, add 80 grams of ethyl 8-halooctanoate containing by-product ethyl 8-ethoxyoctanoate (12% content of ethyl 8-ethoxyoctanoate), raise the temperature to 130°C, and slowly introduce Hydrogen bromide gas was passed through and stirred at this temperature for 5 hours, cooled to below 30°C, washed with 40ml of water, and analyzed by GC, the purity was 96.8%, and the content of ethyl 8-ethoxyoctanoate was 3.1%.

Embodiment 2

[0018] In a 500mL three-necked flask, add 80 grams of ethyl 8-halooctanoate containing by-product ethyl 8-ethoxyoctanoate (12% content of ethyl 8-ethoxyoctanoate), raise the temperature to 150°C, and slowly introduce Hydrogen bromide gas was passed through and stirred at this temperature for 5 hours, cooled to below 30°C, washed with 40ml of water, and analyzed by GC, the purity was 99.1%, and the content of ethyl 8-ethoxyoctanoate was 0.9%.

Embodiment 3

[0020] In a 500mL three-neck flask, add 80 grams of ethyl 8-halooctanoate (14% content of ethyl 8-ethoxyoctanoate) containing by-product ethyl 8-ethoxyoctanoate, raise the temperature to 130°C, and slowly introduce Hydrogen chloride gas was passed through and stirred at this temperature for 5 hours, cooled to below 30°C, washed with 40ml of water, and analyzed by GC, the purity was 97.8%, and the content of ethyl 8-ethoxyoctanoate was 2.2%.

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Abstract

The invention discloses a method for recycling a by-product in a preparation process of ethyl 8-halooctanoate. The method comprises the steps of introducing hydrogen halide gas into ethyl 8-halooctanoate containing the by-product ethyl 8-ethoxyoctanoate and stirring the gas for a reaction at the temperature of 100-160 DEG C. According to the method, hydrogen halide, halogen acid, ethyl 8-ethoxyoctanoate and ethyl 8-halooctanoate are adopted for the reaction, so that the ethyl 8-ethoxyoctanoate is converted into the ethyl 8-halooctanoate, the conditions are mild, and the operation is simple andconvenient. Therefore, the method is suitable for industrial production.

Description

technical field [0001] The invention relates to a method for recycling by-products in the preparation process of ethyl 8-halogenated octanoate. Background technique [0002] Ethyl 8-halogenated octanoate is a common carboxylic acid ester, and it is a very valuable intermediate, widely used in the fields of pesticides, medicines and fine chemicals. The structure is as follows: [0003] [0004] The preparation method of ethyl 8-halooctanoate is reported in EP1384706A1 and CN200810041326.3. The above patents use 1,6-dihalohexane as the starting material, react with diethyl malonate, and then decarboxylate and hydrolyze the ester Ethyl 8-halogenated octanoate was obtained. The above technical process will inevitably produce 8-ethoxy octanoic acid ethyl ester by-product, up to more than 3%. This by-product can be removed by rectification, but because the boiling points of ethyl 8-ethoxyoctanoate and ethyl 8-halogenated octanoate are close, there will be 8-15% of the front ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/63C07C67/307
CPCC07C67/307C07C69/63
Inventor 龙中柱邢领俊晏桂刚禹艳坤安娜蔡畅蔡水洪
Owner 启东东岳药业有限公司
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