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Preparation method of hexafluoroisopropyl methyl ether

A technology of hexafluoroisopropyl methyl ether and hexafluoroisopropanol, which is applied in the field of preparation of hexafluoroisopropyl methyl ether, achieves high reaction yield, mild and controllable reaction conditions, and cheap and easy-to-obtain raw materials Effect

Active Publication Date: 2019-05-31
ZHEJIANG RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method avoids the use of highly toxic raw material dimethyl sulfate, it still needs to be reacted in an autoclave, and the product yield is generally below 80%.

Method used

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  • Preparation method of hexafluoroisopropyl methyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Add 47.6 g (0.25 mol) of cuprous iodide, 51 g (0.37 mol) of sodium trifluoroacetate, and 18.5 g (0.25 mol) of ethyl formate into a 250 mL three-necked flask equipped with a constant pressure dropping funnel, a thermometer and a reflux condenser. ) and 100ml DMF, drain the air in the system, and replace it twice with nitrogen, and heated and stirred to 170°C under the protection of nitrogen, and stirred at 170°C for 2 hours, quickly added 2ml 1M HCl solution, and continued at 170°C React at ℃ for 4 hours, and monitor the reaction process with gas chromatography, stop heating after the reaction is complete, let the reaction solution stand for cooling, filter, add 22.5g (0.25mol) of dimethyl carbonate to the filtrate without purification, 10g (0.25mol) of sodium hydroxide ), magnetically stirred and heated to 90°C for reflux for 4 hours, monitored the reaction process with gas chromatography, after the reaction was complete, left to cool, distilled, and got the fraction wit...

Embodiment 2

[0055]Add 47.6 g (0.25 mol) of cuprous iodide, 48.2 g (0.37 mol) of ammonium trifluoroacetate, and 18.5 g (0.25 mol) and 100ml DMF, drain the air in the system, and replace it twice with nitrogen, and heat and stir to 170°C under the protection of nitrogen, and stir at 170°C for 2 hours, quickly add 2ml 1M HCl solution, continue to React at 170°C for 4 hours, and monitor the reaction process with gas chromatography. After the reaction is complete, stop heating, and the reaction solution is left to cool, filtered, and the filtrate is added without purification. 22.5g (0.25mol) of dimethyl carbonate, 10g (0.25mol) of sodium hydroxide mol), magnetically stirred and heated to 90°C for reflux for 4 hours, monitored the reaction process with gas chromatography, after the reaction was complete, left to cool, distilled, and got the fraction with a boiling point of 50-51°C to obtain 42.8g of product.

[0056] After testing, the product was 1,1,1,3,3,3-hexafluoroisopropanol methyl ether...

Embodiment 3

[0058] Add 47.6 g (0.25 mol) of cuprous iodide, 56.24 g (0.37 mol) of potassium trifluoroacetate, and 18.5 g (0.25 mol) and 100ml DMF, drain the air in the system, and replace it twice with nitrogen, and heat and stir to 170°C under the protection of nitrogen, and stir at 170°C for 2 hours, quickly add 2ml 1M HCl solution, continue to React at 170°C for 4 hours, and monitor the reaction process with gas chromatography. After the reaction is complete, stop heating, and the reaction solution is left to cool, filtered, and the filtrate is added without purification. 22.5g (0.25mol) of dimethyl carbonate, 10g (0.25mol) of sodium hydroxide mol), heated to 90°C with magnetic stirring and refluxed for 4 hours, monitored the reaction process with gas chromatography, after the reaction was complete, left to cool, distilled, and took the fraction with a boiling point of 50-51°C to obtain 42.2g of product.

[0059] After testing, the product was 1,1,1,3,3,3-hexafluoroisopropanol methyl e...

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Abstract

The invention discloses a preparation method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. The preparation method includes reacting trifluoroacetate with formate to obtain 1,1,1,3,3,3-hexafluoroisopropanol, and applying a methylation reagent to the 1,1,1,3,3,3-hexafluoroisopropanol to obtain the 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. The preparation method has the advantages that raw materials are cheap and easy to obtain, the preparation process is mild and the method is simple to operate.

Description

technical field [0001] The invention relates to a preparation method of fluorine-containing ether, in particular to a preparation method of hexafluoroisopropyl methyl ether. Background technique [0002] 1,1,1,3,3,3-Hexafluoroisopropylmethyl ether, English name: Hexafluoroisopropylmethyl ether, abbreviated as "HFE-356mmz", CAS No.13171-18-1, molecular formula C 4 h 4 f 6 O, the molecular weight is 182.06, the boiling point is 50.95°C, the relative density is 1.030-1.038, the refractive index is 1.284, the saturated vapor pressure (25°C) is 36.1k Pa, low toxicity, flammable in case of open flame, low gas thermal conductivity, chemical stability High; combustion produces toxic fluoride fumes. [0003] 1,1,1,3,3,3-Hexafluoroisopropyl methyl ether has an important application in medicine. It can be used as a nerve excitation inhibitor, sedative, anesthetic, and can also be used as an intermediate to synthesize sevoflurane and chlorine Compounds such as fluorine-containing et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/12C07C41/16C07C29/64C07C31/38
Inventor 李伟张迪刘东鹏郭智恺
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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