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Method for preparing chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether

A technology of hexafluoroisopropyl ether and chloromethyl, which is applied in ether preparation, chemical instruments and methods, organic chemistry, etc., can solve the problems of low yield, strong corrosion of equipment, and low purity, and achieve low price, Shorten the reaction time and improve the effect of the original process

Inactive Publication Date: 2010-06-16
JIANGSU HENGRUI MEDICINE CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the yield of the reaction intermediate chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether in this method is relatively low and the purity is not high.
[0006] A recent international patent application, publication number WO2008 / 037039, teaches high purity and high yields of chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl by adding concentrated sulfuric acid or oleum Ether, but concentrated sulfuric acid or oleum is highly corrosive to equipment

Method used

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  • Method for preparing chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add 27.0g (0.20mol) anhydrous AlCl to the 250ml dry three-necked bottle 3 and 8.5g (0.20mol) LiCl, cool to -5°C with stirring, add 20.5ml (0.20mol) 1,1,1,3,3,3-hexafluoro-2-propanol dropwise (dropping time 10 minutes) . After dropping, stirring was continued for 15 minutes, 9.0 g (0.30 mol) of paraformaldehyde was added, the cooling bath was removed, and the white mixture was stirred at room temperature for 8 hours. After the reaction was completed, the temperature was lowered to -5°C, 100 ml of 5N hydrochloric acid and 20 ml of water were added dropwise, and the mixture was stirred for 1 hour and then left to stand. The organic phase (lower layer) was separated to obtain 37.9 g of a colorless liquid with a yield of 88.1%. Its purity was 99.3% by gas chromatography.

Embodiment 2

[0023] Add 27.0g (0.20mol) anhydrous AlCl to the 250ml dry three-necked bottle 3 , cooled to -5°C with stirring, and 20.5 ml (0.20 mol) of 1,1,1,3,3,3-hexafluoro-2-propanol was added dropwise (dropwise addition time 10 minutes). Then 28.4 ml (0.40 mol) of thionyl chloride were added dropwise. After dropping, stirring was continued for 15 minutes, 9.0 g (0.30 mol) of paraformaldehyde was added, the cooling bath was removed, and the white mixture was stirred at room temperature for 6 hours. After the reaction was completed, the temperature was lowered to -5°C, 100 ml of 5N hydrochloric acid and 40 ml of water were added dropwise, and the mixture was stirred for 1 hour and then left to stand. The organic phase (lower layer) was separated to obtain 37.2 g of a colorless liquid with a yield of 87.2%. Its purity was 98.2% by gas chromatography.

Embodiment 3

[0025] Add 27.5g (0.20mol) anhydrous PCl to the 250ml dry three-necked bottle 3 and 0.75g (0.01mol) KCl, cool to -5°C with stirring, add 20.5ml (0.20mol) 1,1,1,3,3,3-hexafluoro-2-propanol dropwise (dropwise addition time 10 minutes) . After dropping, stirring was continued for 15 minutes, 9.0 g (0.30 mol) of paraformaldehyde was added, the cooling bath was removed, and the white mixture was stirred at room temperature for 8 hours. After the reaction was completed, the temperature was lowered to -5°C, 150 ml of 5N hydrochloric acid and 20 ml of water were added dropwise, and the mixture was stirred for 1 hour and then left to stand. The organic phase (lower layer) was separated to obtain 37.9 g of a colorless liquid with a yield of 88.1%. Its purity was 99.3% by gas chromatography.

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Abstract

The invention relates to a method for preparing chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether. 1,1,1,3,3,3-hexafluoro-2-propanol and 1,3,5-trioxane or oligomeric formaldehyde react in a binary catalyst system which takes anhydrous chlorinated Lewis acid as a main catalyst and a chloric compound as an auxiliary catalyst to form the chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether. The method has the advantages of utilizing the low-cost binary catalyst system, greatly improving the prior art, shortening reaction time and greatly increasing the yield of chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether. The chloromethyl-1,1,1,3,3,3-hexafluoro isopropyl ether has the purity up to over 98 percent and the yield up to over 87 percent.

Description

technical field [0001] The present invention relates to a method for preparing hexafluoroisopropyl ether, in particular a method for preparing chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, which consists of 1,1,1,3, 3,3-hexafluoro-2-propanol and 1,3,5-trioxane or paraformaldehyde in a binary catalytic system with anhydrous chlorinated Lewis acid as main catalyst and chlorine-containing compound as co-catalyst The reaction occurred in chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether. technical background [0002] Chloromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether is an important intermediate in the synthesis of fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether . The latter molecular formula (CF 3 ) 2 CHOCH 2 F, referred to as sevoflurane. In recent years, studies have found that sevoflurane has the properties of inducing anesthesia and quick recovery, and can also reduce cerebral vascular resistance, cerebral metabolic rate, cerebral oxygen consumption, myocard...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/01B01J27/08B01J27/14
CPCC07C41/01
Inventor 孙飘扬童达君李迎宾卢长娟刘潇梅杰
Owner JIANGSU HENGRUI MEDICINE CO LTD