Preparation method of 2,2-difluoroethanol

A technology of difluoroethanol and difluoroacetyl halide is applied in the field of preparing 2,2-difluoroethanol, can solve the problems of high cost, low reaction yield, low yield and the like, achieves mild reaction conditions, simple process steps, high yield effect

Pending Publication Date: 2020-08-07
SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Among the above preparation methods, the difluoroacetyl chloride gas-phase catalyst reduction method must use noble metals, which is costly and has the problem of easy deactivation of the noble metal catalyst, and 1,1-difluoro-2-bromo (or chloro)ethane must use high pressure and high temperature reaction conditions, and the reaction yield is low, the raw material of difluoroacetic acid (ester) liquid phase reduction method is not easy to get, the production cost is high, and the yield is not high

Method used

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  • Preparation method of 2,2-difluoroethanol

Examples

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Effect test

Embodiment 1

[0042] Add 22.6g (0.6mol) of NaBH to a 1000ml reactor with magnetic stirring, thermocouple and cooling coil 4 , then add 200ml of CH 3 Oh. Stir and keep the temperature of the reactor at about -10°C, slowly feed 98.0g (1.0mol) of CF into the reactor 2 HCOF, keep the reaction temperature at -10~0℃, wait for CF 2 After the addition of HCOF, continue to stir for 1.0 h, add hydrochloric acid to adjust the pH value of the still liquid to 3-4, and terminate the reaction. The still liquid was subjected to a rectification operation to obtain the product 2,2-difluoroethanol with a yield of 96.1%.

Embodiment 2

[0044] Add 11.4g (0.3mol) of LiAlH to a 1000ml reactor with magnetic stirring, thermocouple and cooling coil 4 and 300ml of diethylene glycol dimethyl ether, stir and keep the still temperature of the reaction kettle at about -10°C. Slowly feed 58.8g (0.6mol) of CF into the reactor 2HCOF, keep the kettle temperature at about -10~0℃, wait for CF 2 After the addition of HCOF, continue to stir for 0.5h, add hydrochloric acid to adjust the pH value of the kettle liquid to 2-3, and terminate the reaction. The still liquid was subjected to a rectification operation to obtain the product 2,2-difluoroethanol with a yield of 97.8%.

Embodiment 3

[0046] NaBH 4 and substrate CF 2 The molar ratio of HCOF was changed to 0.5:1, and all the other operating conditions were the same as in Example 1. After the reaction, the still liquid was rectified to obtain the product 2,2-difluoroethanol with a yield of 91.2%.

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Abstract

The invention discloses a preparation method of 2,2-difluoroethanol. 2,2-difluoroethanol is obtained by liquid-phase one-step reaction of 2,2-difluoroacetyl halide and a metal hydride. The method provided by the invention has the advantages of high product yield, simple reaction steps, mild reaction conditions and the like.

Description

technical field [0001] The invention relates to a method for preparing 2,2-difluoroethanol. Background technique [0002] 2,2-Difluoroethanol is an important aliphatic fluorine-containing intermediate, which is widely used in the synthesis of pesticides, medicines and fluoropolymers, and can be used in the synthesis of herbicides and insecticides in the field of pesticides, such as Penoxsulam can be used in the field of medicine to construct difluoroethoxy groups, and the resulting drugs can be used as mPGE synthase inhibitors, PDE-4 inhibitors, retinoid X receptor regulators and muscarinic receptors In the field of fluorine-containing polymers, difluoroethoxy groups can be introduced into the molecule through reactions to improve the performance of the polymer. For example, the monomer-methyl Difluoroethyl acrylate. [0003] For the preparation method of 2,2-difluoroethanol, difluoroacetyl chloride, 1,1-difluoro-2-bromo (or chloro)ethane, difluoroacetic acid or difluoroac...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/147C07C31/38
CPCC07C29/147C07C31/38
Inventor 马立博许磊杨会娥刘坤峰任昊曾昌华甄文萃
Owner SINOCHEM MODERN ENVIRONMENTAL CHEM INDAL XI ANCO
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