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Method for catalytically hydrogenating difluoroacetic acid

A technology for catalytic hydrogenation of difluoroacetic acid and difluoroacetic acid, which can be used in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as uneconomical application

Inactive Publication Date: 2012-07-04
SHANGHAI SINOFLUORO SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these synthetic routes are not economically applicable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 35ml of toluene solution of 11g of sodium borohydride into a reaction kettle containing 150ml of toluene, seal the reaction kettle and fill it with nitrogen, add 100g of difluoroacetic acid when the temperature rises to 40 degrees Celsius, and keep the reaction for 2 hours. Add 300ml of water, recover toluene by distillation, adjust the pH value to 2-3 with 20% hydrochloric acid, then adjust the pH value to 10 with 25% sodium bicarbonate solution, filter, and dry to obtain 97 g of difluoroethanol with a yield of 89%.

Embodiment 2

[0018] Add 50ml of toluene solution of 15g of sodium borohydride into a reaction kettle containing 150ml of toluene, seal the reaction kettle and fill it with nitrogen, add 150g of difluoroacetic acid when the temperature rises to 50 degrees Celsius, and keep the reaction for 2 hours. Add 500ml of water, recover toluene by distillation, adjust the pH value to 2-3 with 20% hydrochloric acid, then adjust the pH value to 10 with 25% sodium bicarbonate solution, filter, and dry to obtain 123 g of difluoroethanol with a yield of 88%.

Embodiment 3

[0020] Add 80ml of toluene solution of 20g of sodium borohydride into a reaction kettle containing 250ml of toluene, seal the reaction kettle and fill it with nitrogen, add 150g of difluoroacetic acid when the temperature rises to 45 degrees Celsius, and keep the reaction for 2 hours. Add 400ml of water, recover toluene by distillation, adjust the pH value to 2-3 with 20% hydrochloric acid, then adjust the pH value to 10 with 25% sodium bicarbonate solution, filter, and dry to obtain 177 g of difluoroethanol, with a yield of 86%.

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Abstract

The invention relates to a method for catalytically hydrogenating difluoroacetic acid. The new method includes the following steps: step 1: preparation of catalyst: sodium borohydride as catalyst is added into organic solvent solution; step2: implementation of main reaction: the organic solvent with the sodium borohydride is added into a reaction kettle, the reaction kettle is sealed, temperature is increased, the difluoroacetic acid is added, and after sufficient reaction, the temperature is kept; step 3: extraction and rectification of product: the reaction product in step 2 is added with 300ml of water, the organic solvent is recovered by distillation, hydrochloric acid is used for regulating the pH value to 2 to 3, sodium bicarbonate solution is then used for regulating the pH value to 10, and after filtration and drying, product is obtained.

Description

technical field [0001] The invention relates to the field of fluorine chemical industry, in particular to a method for catalytically hydrogenating difluoroacetic acid. Background technique [0002] Difluoroethanol is an alcohol used in organic synthesis, especially in the fields of agrochemical and pharmaceutical. Various methods for the synthesis of difluoroethanol have been proposed. [0003] For example, Chinese Patent No. 200680047867.6, which relates to a new method for preparing difluoroethanol. The process for the preparation of difluoroethanol according to the invention comprises the hydrogenation of acetyl halides according to the following formula (I) in the presence of an effective amount of a catalyst comprising at least one element of the periodic table deposited on a solid inorganic support having acidic properties Group VIII element: In formula (I), X represents a halogen atom other than a fluorine atom. In particular difluoroacetyl chloride can be reduced ...

Claims

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Application Information

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IPC IPC(8): C07C31/38C07C29/147
Inventor 江静朱虹
Owner SHANGHAI SINOFLUORO SCI
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