Preparation of 2,2,2- trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether

A technology of hexafluoropropyl ether and trifluoroethyl, applied in the field of preparation of 2,2,2-trifluoroethyl 1,1,2,3,3,3-hexafluoropropyl ether, can solve Palladium is expensive, not suitable for large-scale industrial production, and has toxicity, etc., to achieve the effect of convenient post-processing, mild conditions, and low price

Inactive Publication Date: 2013-10-23
SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the above reactions all need to be operated under pressure. The catalyst 18-C-6 and tetrakistriphenylphosp

Method used

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  • Preparation of 2,2,2- trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether
  • Preparation of 2,2,2- trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether

Examples

Experimental program
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Effect test

Embodiment 1

[0022] The preparation of CF3CH2OCF2CHFCF3 under the optimal conditions of embodiment 1

[0023] Take 330ml of DMF and add it into a three-necked flask, add 5.3g of KF and 25g of tetrabutylammonium chloride into it and stir to dissolve. Add 330ml CF3CH2OH, then pass through perfluoropropene gas, and control the reaction temperature to 40°C with an oil bath until the reaction is complete. After post-treatment, rectification under normal pressure to obtain the final product 2,2,2-trifluoroethyl 1,1,2,3,3,3-hexafluoropropyl ether with a boiling point of 71.5-73°C and a purity of 99.7%. Yield 70-80%.

Embodiment 2

[0024] The preparation of CF3CH2OCF2CHFCF3 under embodiment 2KF catalyzed acetonitrile as solvent condition

[0025] Weigh 0.04g KF into a three-necked flask, add 60ml of acetonitrile and stir to dissolve, then add 7.2ml of CF3CH2OH, pass perfluoropropylene gas to evacuate the air, and then pass perfluoropropylene gas to react at 40°C under airtight conditions. There are surplus raw materials, and the yield is 40-50%.

Embodiment 3

[0026] The preparation of CF3CH2OCF2CHFCF3 under embodiment 3KF catalyzed DMF as solvent condition

[0027] As in the method of Example 2, 0.04g KF, 60ml acetonitrile and 7.2ml CF3CH2OH were weighed for reaction. There are surplus raw materials, and the yield is 40-50%.

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Abstract

The invention relates to a preparation method of 2,2,2-trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether. Trifluoroethanol reacts with hexafluoropropylene in an organic polar solvent and in the presence of potassium fluoride and phase-transfer catalyst, at the temperature of room temperature to 50 DEG C, so as to produce 2,2,2- trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether, and the phase-transfer catalyst is 18-crown-6, tetrabutylammonium chloride or trimethylphenylammonium. The preparation method of 2,2,2- trifluoroethyl-1,1,2,3,3,3-hexafluoroisopropyl ether has the advantages of mild reaction conditions, normal pressure reaction, low catalyst price, convenient post-treatment, and good yield and selectivity, and is suitable for industrial production.

Description

technical field [0001] The invention relates to the preparation of 2,2,2-trifluoroethyl 1,1,2,3,3,3-hexafluoropropyl ether. Background technique [0002] Hydrofluoroethers (HFEs) have no damage to the ozone layer (ODP=0), low greenhouse effect (low GWP value), and good physical and chemical properties, such as low surface tension, non-combustibility, excellent solubility, etc. These compounds are considered to be the third-generation ODS substitutes with the most potential to replace chlorofluorocarbons (CFCs) and hydrofluorocarbons (HCFCs) as refrigerants, cleaning agents, and blowing agents. Among them, 2,2,2-trifluoroethyl 1,1,2,3,3,3-hexafluoropropyl ether (HFE-449) has the advantages of non-explosion and moderate boiling point due to its high fluorine content , is an ideal candidate compound to replace ODS. [0003] There are not many reports on the preparation of 2,2,2-trifluoroethyl 1,1,2,3,3,3-hexafluoropropyl ether in the literature. In 2008, Debby Natalia et al. ...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/06
Inventor 吴永明高源
Owner SHANGHAI INST OF ORGANIC CHEM CHINESE ACAD OF SCI
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