A process for the preparation of ethyl difluoroacetate

By reacting 2,2-difluoro-1,1-dichloroethyl ether with concentrated sulfuric acid to generate a sulfate ester compound and then hydrolyzing it, the harsh reaction conditions and scarce raw materials in the synthesis of ethyl difluoroacetate were solved, and a high-yield and environmentally friendly preparation method was achieved.

CN115368236BActive Publication Date: 2025-11-04JIANGSU BLUESTAR GREEN TECH
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Patent Information

Application Number
CN202211152366.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-09-21
Publication Date
2025-11-04
Estimated Expiration
2042-09-21

AI Technical Summary

Technical Problem

Existing methods for synthesizing ethyl difluoroacetate suffer from problems such as harsh reaction conditions, numerous side reactions, poor product selectivity, difficulty in obtaining raw materials, low reaction yield, and environmental unfriendliness.

Method used

2,2-Difluoro-1,1-dichloroethyl ether was reacted with concentrated sulfuric acid at a certain temperature to generate a sulfate ester compound, which was then hydrolyzed. By controlling the reaction temperature and concentration, ethyl difluoroacetate was obtained.

Benefits of technology

It achieves a simple process, readily available raw materials, mild reaction conditions, high product yield, and few by-products, making it suitable for industrial production and reducing raw material loss and environmental impact.

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Abstract

The application relates to the technical field of organic synthesis, in particular to a preparation method of ethyl difluoroacetate, which comprises the following steps: S1, 2,2-difluoro-1,1-dichloroethyl ethyl ether is added into a reaction kettle, concentrated sulfuric acid is added dropwise under stirring at a certain reaction temperature, after the dropwise addition is completed, the reaction is continuously kept for reaction completion, and a compound shown in formula I is obtained; S2, water is added into a reaction container, the compound shown in formula I prepared in the step S1 is added dropwise into the reaction container for hydrolysis reaction at a certain temperature, after the reaction is completed, the reaction is allowed to stand and is separated into layers, and the lower organic layer is ethyl difluoroacetate; the application has the advantages of simple process, easily obtained raw materials, mild reaction conditions, easy control, high product yield, few by-products, reaction condition detection at any time, one-time reaction completion, secondary recovery treatment avoidance, raw material loss reduction and easy industrialized production.
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