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Process method for catalytic synthesis of 1,1,1,3,3,3-hexafluoro isopropyl methyl ether

A process method and technology of hexafluoroisopropanol, applied in catalytic synthesis 1, can solve problems such as low process yield and purity, and achieve the effect of improving yield and purity

Inactive Publication Date: 2016-07-13
LIANYUNGANG TETRAFLUOR NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention discloses a new method for catalytically synthesizing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether, using dimethyl sulfate and hexafluoroisopropanol as raw materials in an alkaline environment , preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether under the action of a soluble quaternary ammonium salt phase transfer catalyst, which solved the problem of low yield and purity in the existing process

Method used

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  • Process method for catalytic synthesis of 1,1,1,3,3,3-hexafluoro isopropyl methyl ether
  • Process method for catalytic synthesis of 1,1,1,3,3,3-hexafluoro isopropyl methyl ether

Examples

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Effect test

Embodiment 1

[0022] In a 250 ml four-necked flask equipped with reflux condenser, stirrer, constant pressure titration funnel, and thermometer, add quantitative water, 0.02mol tetrabutylammonium bromide, 1mol hexafluoroisopropanol, and stir to make phase transfer agent IV Butylammonium bromide is completely dissolved. Lower the temperature, slowly add lye solution dropwise, react for 1 hour, keep the temperature constant, drop 1.2 mol of dimethyl sulfate, adjust the temperature to 25-30°C, and react for 4 hours. Add lye and dimethyl sulfate, and continue the reaction for 3 hours. After the reaction is completed, the aqueous layer is removed, the organic phase is washed with lye, anhydrous magnesium sulfate is added to dry, and the 51-52°C fraction is collected by atmospheric distillation. The purity is 99.87% determined by FID.

[0023] The above process can be summarized as specific steps under the premise of the basic preparation process, that is, in step (1), 0.02 mol of tetrabutylammoniu...

Embodiment 2

[0025] In a 250ml four-necked flask equipped with reflux condenser, stirrer, constant pressure titration funnel and thermometer, add quantitative water, 0.01mol tetrabutylammonium bromide, 1mol hexafluoroisopropanol, stir to make phase transfer agent IV Butylammonium bromide is completely dissolved. Lower the temperature, slowly add lye solution dropwise, react for 1 hour, keep the temperature constant, drop 1.4 mol of dimethyl sulfate, adjust the temperature to 25-30°C, and react for 3 hours. Add lye and dimethyl sulfate, and continue the reaction for 1 hour. After the reaction is completed, the aqueous layer is removed, the organic phase is washed with lye, dried by adding anhydrous magnesium sulfate, and distilled under normal pressure to collect the fraction at 51-52°C. The purity is determined to be 99.5%.

[0026] The above process can be summarized as the specific steps under the premise of the basic preparation process, that is, in step (1), 0.01 mol of tetrabutylammoniu...

Embodiment 3

[0028] In a 250 ml four-necked flask equipped with reflux condenser, stirrer, constant pressure titration funnel and thermometer, add quantitative water, 0.04mol tetrabutylammonium bromide, 1mol hexafluoroisopropanol, and stir to make phase transfer agent IV Butylammonium bromide is completely dissolved. Lower the temperature, slowly add lye solution dropwise, react for 2 hours, keep the temperature constant, drop 1.3 mol of dimethyl sulfate, adjust the temperature to 25-30°C, and react for 2 hours. Add lye and dimethyl sulfate, and continue the reaction for 2 hours. After the reaction is completed, the aqueous layer is removed, the organic phase is washed with lye, anhydrous magnesium sulfate is added to dry, and the 51-52°C fraction is collected by atmospheric distillation. The purity is determined to be 99.6%.

[0029] The above process can be summarized as a specific step under the premise of the basic preparation process, that is, in step (1), 0.04 mol of tetrabutylammonium...

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Abstract

The present invention relates to a process method for catalytic synthesis of 1,1,1,3,3,3-hexafluoro isopropyl methyl ether, and the method includes the steps of preparation of an alkaline hexafluoroisopropanol solution containing a phase transfer catalyst, preparation of hexafluoro isopropyl methyl ether, distillation and purification and the like. The 1,1,1,3,3,3-hexafluoro isopropyl methyl ether is prepared from dimethyl sulfate and hexafluoroisopropanol as raw materials in an alkaline environment under the effect of a soluble quaternary ammonium salt phase transfer catalyst, and product yield and purity are greatly improved.

Description

Technical field [0001] The present invention relates to a preparation process of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether, in particular to a method for synthesizing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether using a phase transfer catalyst Process method of fluoroisopropyl methyl ether. Background technique [0002] 1,1,1,3,3,3-hexafluoroisopropyl methyl ether is the key raw material for the synthesis of fluorinated anesthetics sevoflurane. Sevoflurane is a new type of inhaled anesthetic with significantly lower irritation to the respiratory tract Compared with other inhaled anesthetics, it has the characteristics of inducing anesthesia and quick recovery, and the market prospect is promising. [0003] The US patent document with publication number US5705710 discloses a scheme for preparing 1,1,1,3,3,3-hexafluoroisopropyl methyl ether called PROCESSFORTHESYNTHESISOFHEXAFLUOROISOPROPYLETHERS, which uses α,α-dicyanomethyl Methyl methyl ether and bromine trifluoride are raw m...

Claims

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Application Information

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IPC IPC(8): C07C43/12C07C41/16
Inventor 吕志强姚洪星
Owner LIANYUNGANG TETRAFLUOR NEW MATERIALS
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