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Method for preparing 2,2-difluoroethanol from 2,2-difluoro-1-halogenated ethane

A technology of halogenated ethane and difluoroethanol, which is applied in the field of preparation of 2,2-difluoroethanol, can solve the problems of high cost of raw materials, high cost of industrialized production, and difficult to handle, and achieves reduction of production cost and simplification of industrial production. Process, the effect of reducing the amount of production

Active Publication Date: 2016-01-13
HUBEI HAIZHIJIE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technology disclosed in the above patent has an obvious defect, the process flow is long, and the solid waste generated is much and difficult to handle. Therefore, the cost of industrial production is relatively high
Other technical routes such as the reduction of difluoroacetic acid carboxylate to prepare difluoroethanol are economically inadvisable due to the long process route and high cost of raw materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] 100.5 g (1 mol) of 2,2-difluoro-1-chloroethane, 60 g of sodium hydroxide, 0.5 g of sodium iodide and 140 g of sulfolane with a water content of 1000 ppm were first charged into the autoclave. The reaction mixture was heated to 200° C. and stirred at this temperature for 10 hours. Then, the temperature was lowered to 120° C., and the reaction mixture was distilled to obtain the target product: 2,2-difluoroethanol; the yield was 87%.

[0021] Yield is defined as follows:

[0022] The yield is defined as the mole percentage of the main raw material converted to the target product.

Embodiment 2

[0024] 100.5g (1mol) of 2,2-difluoro-1-chloroethane, 60g of sodium hydroxide, 0.5g of sodium iodide and 140g of N,N-dibutylformamide with a water content of 800ppm were first charged into the autoclave. The reaction mixture was heated to 195°C and the reaction was stirred at this temperature for 10 hours. Then, the temperature was lowered to 120° C., and the reaction mixture was distilled to obtain the target product: 2,2-difluoroethanol; the yield was 86%.

Embodiment 3

[0026] 100.5g (1mol) of 2,2-difluoro-1-chloroethane, 60g of sodium hydroxide and 140g of sulfolane with a water content of 1000ppm were first charged into the autoclave. The reaction mixture was heated to 200°C and the reaction was stirred at this temperature for 12 hours. Then, the temperature was lowered to 120° C., and the reaction mixture was distilled to obtain the target product: 2,2-difluoroethanol; the yield was 81%.

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PUM

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Abstract

The invention discloses a method for preparing 2,2-difluoroethanol from 2,2-difluoro-1-halogenated ethane, which comprises the following steps: in the presence of a catalyst, reacting 2,2-difluoro-1-halogenated ethane with alkali metal hydroxide in a solvent, and collecting the 2,2-difluoroethanol from the reaction product. The method simplifies the industrial production process, lowers the production cost, reduces the solid waste generation quantity, and implements the clean production.

Description

technical field [0001] The invention relates to a preparation method of 2,2-difluoroethanol. Background technique [0002] 2,2-Difluoroethanol is an important intermediate in the synthesis of important agricultural chemical and pharmaceutical active substances, especially for the preparation of penoxsulam, a broad-spectrum herbicide with high efficiency, low toxicity and easy degradation. At present, many patents and documents have reported their respective technologies for preparing the 2,2-difluoroethanol, such as the technology disclosed in Chinese Patent Application No. 2012800356104. The technology disclosed in this patent includes the following steps: (i): 1-chloro-2,2-difluoroethane reacts with formic acid or acetic acid alkali metal salt in a suitable solvent to generate the corresponding 2,2-difluoroethyl formate or 2,2-bis Fluoroethyl acetate, characterized in that 1-chloro-2,2-difluoroethane is slowly added to a mixture of solvent and an alkali metal salt of form...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C31/38C07C29/124
CPCC07C29/124C07C31/38
Inventor 王忠平刘纯山
Owner HUBEI HAIZHIJIE CHEM