Preparation method of hexafluoroisopropyl methyl ether
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A technology of hexafluoroisopropyl methyl ether and hexafluoroisopropanol, applied in 1 field, can solve the problems of high operating cost, low product yield and the like
Active Publication Date: 2012-04-11
SINOCHEM LANTIAN +1
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[0005] (1) U.S. Patent US3346448 and British Patent GB1250928 have reported the use of dimethyl sulfate to react with hexafluoroisopropanol under the effect of alkali, and the method is more convenient to synthesize hexafluoroisopropyl methyl ether, but the product yield is not high High, and the use of highly toxic raw materials at the same time puts forward higher requirements for the
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[0021] Example 1
[0022] Add raw material hexafluoroisopropanol 70g, sodium hydroxide 15g, solvent acetonitrile 60g into a 0.25L pressure reactor, heat up to 40°C after mixing, slowly add 50g methyl iodide while stirring, keep constant temperature for 6 hours, and the reaction ends After cooling down, 52.7 g of the product hexafluoroisopropyl methyl ether was obtained by distillation, and the product yield was 82.3%.
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[0023] Example 2
[0024] Add 70g of raw material hexafluoroisopropanol, 20g of potassium hydroxide, and 50g of solvent dimethyl sulfoxide into a 0.25L pressure reactor, heat up to 50°C after mixing, slowly add 30g of methyl bromide under stirring, and react at constant temperature for 6 hours , Distilled after the reaction to obtain the product hexafluoroisopropyl methyl ether 43g, the product yield was 74.1%.
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[0025] Example 3
[0026] Add 80g of raw material hexafluoroisopropanol, 20g of sodium hydroxide, 60g of solvent N,N-dimethylformamide into a 0.25L pressure reactor, heat up to 60°C after mixing, and slowly add 40g of methyl chloride under stirring , constant temperature reaction for 6 hours, cooling down after the reaction, distillation to obtain the product hexafluoroisopropyl methyl ether 58.7g, product yield 67.7%.
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Abstract
The invention discloses a preparation method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. In the preparation method, hexafluoroisopropyl alcohol and halogenated methane are taken as raw materials to synthesize the 1,1,1,3,3,3-hexafluoroisopropyl methyl ether under the action of a base catalyst, wherein, the halogenated methane has the following general formula: CH3X, wherein, X is chosen from Cl, Br or I. The preparation method has the advantages of available raw materials and mild preparation process, and is simple in operation; and the obtained 1,1,1,3,3,3-hexafluoroisopropyl methyl ether can be taken as an intermediate to synthesize the methyl fluoride-1,1,1,3,3,3- hexafluoroisopropyl ether.
Description
technical field [0001] The invention relates to a preparation method of 1,1,1,3,3,3-hexafluoroisopropyl methyl ether. Background technique [0002] 1,1,1,3,3,3-Hexafluoroisopropyl methyl ether, CAS registration number: 13171-18-1, molecular formula C 4 h 4 f 6 O, with a molecular weight of 182.06, a boiling point of 50.9°C, a relative density of 1.030-1.038, a refractive index of 1.284, a saturated vapor pressure (25°C) of 36.1KPa, low toxicity, flammable in case of an open flame, a gas with low thermal conductivity and high chemical stability high. It is the key raw material for the synthesis of fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl ether, while fluoromethyl-1,1,1,3,3,3-hexafluoroisopropyl Commonly known as sevoflurane or sevoflurane, base ether is a new type of inhaled general anesthetic, clinically characterized by short anesthesia and recovery time, less toxic and side effects on the kidneys, and reduced cerebrovascular pressure, brain metabolism, and brain ox...
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