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Synthesis method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether

A synthesis method and technology of hexafluoroisopropanol, applied in 1 field, can solve problems such as low product yield, and achieve the effects of reducing investment and cost, good economic benefits, and high yield

Active Publication Date: 2012-07-18
SANMING HEXAFLUO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method of synthesizing hexafluoroisopropyl methyl ether is relatively simple and easy to implement, but due to the use of highly toxic dimethyl sulfate, higher requirements are placed on the operating environment and wastewater treatment, and it is easier to cause problems in environmental protection and safety. , and the product yield is also low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a 2-liter stainless steel autoclave with stirring and electric heating, add 500 grams of hexafluoroisopropanol, 1200 grams of dimethyl carbonate, and 200 grams of potassium carbonate. All valves were turned on for heating and stirring, and the temperature in the kettle was raised to 180° C., and reacted at this temperature for 5 hours. After the reaction, lower the temperature of the kettle to normal temperature, remove the residual pressure in the kettle, release the reaction liquid, filter out the insoluble solids, then put it in a glass distillation tower for distillation, take the fraction with a boiling point of 50-51°C, and obtain 480 grams of product , was identified as hexafluoroisopropyl methyl ether by gas chromatography, and its purity was determined to be 99.6%. The yield is 88.6%.

Embodiment 2

[0024] In a 2-liter stainless steel autoclave with stirring and electric heating, add 500 grams of hexafluoroisopropanol, 1200 grams of dimethyl carbonate, and 200 grams of powdered basic alumina. Air, then close all valves, turn on heating and stirring, raise the temperature in the kettle to 190°C, and react at this temperature for 5 hours. After the reaction, lower the temperature of the kettle to normal temperature, remove the residual pressure in the kettle, release the reaction liquid, filter out the insoluble solids, then put it in a glass distillation tower for distillation, take the fraction with a boiling point of 50-51°C, and obtain 495 grams of product , calibrated by gas chromatography to be hexafluoroisopropyl methyl ether, and its purity was determined to be 99.8%. The yield is 91.3%.

[0025] Example 2:

[0026] In a 2-liter stainless steel autoclave with stirring and electric heating, add 500 grams of hexafluoroisopropanol, 1200 grams of dimethyl carbonate, a...

Embodiment 3

[0028] In a 2-liter stainless steel autoclave with stirring and electric heating, add 400 grams of hexafluoroisopropanol, 1300 grams of dimethyl carbonate, and 200 grams of powdered basic alumina. Air, then close all valves, turn on heating and stirring, raise the temperature in the kettle to 210°C, and react at this temperature for 3 hours. After the reaction, lower the temperature of the kettle to normal temperature, remove the residual pressure in the kettle, release the reaction liquid, filter out the insoluble solids, then put it in a glass distillation tower for distillation, take the fraction with a boiling point of 50-51°C, and obtain 515 grams of product , calibrated by gas chromatography to be hexafluoroisopropyl methyl ether, and its purity was determined to be 99.5%. The yield was 95.0%.

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PUM

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Abstract

The invention discloses a synthesis method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. The method comprises the following steps: adding hexafluoroisopropanol, methyl carbonate and alkali catalyst in a reactor to carry out reaction at a temperature of between 100 and 300 DEG C for 0.5 to 10 hours; and then obtaining the product after cooling, filtration and distillation. Due to adopting the methyl carbonate and alkali catalyst, the synthesis method has great significance to environmental protection and safe production and obtains the product with high purity and high yield; moreover, the obtained product also has high storage degree and use stability.

Description

technical field [0001] The invention relates to a synthesis method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. Background technique [0002] Sevoflurane, also known as sevoflurane, is fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, molecular formula (CF 3 ) 2 CHOCH 2 F, is a new type of inhaled general anesthetic, which has the characteristics of induction of anesthesia and rapid recovery, and can also reduce cerebrovascular pressure, cerebral metabolic rate, cerebral oxygen consumption, myocardial contractility and blood pressure, and has obvious irritation to the respiratory tract It is lower than other inhalational anesthetics, and the most important thing is that there is no obvious liver and kidney toxicity in clinical practice, so it has received extensive attention and attention in the world, and has basically replaced its predecessors in developed countries such as desflurane, isoflurane Fluoroethers have also been used more and more clinically in my countr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C43/12C07C41/16B01J27/232B01J21/10B01J23/02B01J21/04B01J31/02
Inventor 王陈锋
Owner SANMING HEXAFLUO CHEM CO LTD
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