Preparation method of 2, 2-difluoroethanol

A technology of difluoroethanol and ethyl difluoroacetate is applied in the field of preparation of 2,2-difluoroethanol, and can solve the problems of low yield, decrease in total yield, increase production cost and the like, and achieve reduction in production cost, Emission reduction effect

Inactive Publication Date: 2014-10-15
南通得宝氟化学有限公司 +1
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  • Abstract
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  • Application Information

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Problems solved by technology

[0005] Using 1,1-difluoro-2-bromo (or chloro)ethane as a raw material, there are many reaction steps and a long time, resulting in a decrease in its total yield
[0006] Using difluoroacetyl chloride as the starting material is the main method of industrial production at present, the reaction reagent is easy to obtain, and the catalyst can be recycled; but the catalyst is expensive and the yield is not high, which increases the production cost
[0007] Using difluoroacetic acid or difluoroacetic acid ester as the starting material, the reaction is relatively simple, especially when difluoroacetic

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  • Preparation method of 2, 2-difluoroethanol
  • Preparation method of 2, 2-difluoroethanol

Examples

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[0025] Implementation examples

[0026] · In a 2000 mL three-necked flask, 38.0 g (1.0 mol) of LiAlH4 was dissolved in 800 mL of tetrahydrofuran. The system was cooled to -10°C in an ice bath, stirred vigorously, and 248 g (2.0 mol) of ethyl difluoroacetate was slowly dropped into the three-neck flask. After the dropwise addition is completed, react for 1 hour, and nuclear magnetic F spectroscopy confirms that the conversion is complete. Use 2mol / L hydrochloric acid to adjust the pH to about 3 to terminate the reaction. The crude product of difluoroethanol can be obtained by distillation.

[0027] · In a 2000 mL three-necked flask, 38.0 g (1.0 mol) of LiAlH4 was dissolved in 800 mL of ethylene glycol dimethyl ether. The system was cooled to -10°C in an ice bath, stirred vigorously, and 248 g (2.0 mol) of ethyl difluoroacetate was slowly dropped into the three-necked flask. After the dripping is completed, react for 1 hour, and nuclear magnetic F spectroscopy confirms that the con...

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Abstract

The invention provides a preparation method of 2, 2-difluoroethanol. The preparation method comprises the steps as follows: when an organic solution is neutralized to the temperature of subzero 20 DEG C-0 DEG C, methyl difluoroacetate or ethyl difluoroacetate is taken as a raw material, lithium aluminum hydride is taken as a reducing agent, and high-yield and high-purity 2, 2-difluoroethanol is obtained. The method is simple and convenient and can be applicable to large-scale industrial production, and the raw material is easy to obtain.

Description

technical field [0001] The invention relates to a preparation method of 2,2-difluoroethanol, which is a method capable of adapting to large-scale industrial production of 2,2-difluoroethanol. Background technique [0002] After decades of hard work, organic fluorine chemical industry has established a good foundation and scale in my country, and the production scale of some fluorine-containing basic raw materials is already the first in the world, such as: anhydrous hydrofluoric acid, HCFC-22, HFC-134a, tetrafluoroethylene monomer, hexafluoropropylene, etc. Fluorine-containing fine chemical products are an important branch of organic fluorine chemicals. Due to their variety, high added value and high technical content, they are attracting more and more investment interest from production enterprises. Among them, aliphatic fluorine-containing intermediates can be used in the synthesis of surfactants, fabric finishing agents, new pharmaceutical and pesticide synthetic raw mate...

Claims

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Application Information

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IPC IPC(8): C07C31/38C07C29/147
CPCC07C29/147C07C31/38
Inventor 吴永明袁亚芬
Owner 南通得宝氟化学有限公司
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