Preparation method for methyl heptafluoroisobutyrate

A technology of methyl heptafluoroisobutyrate and dimethyl carbonate, applied in the field of organic synthesis, can solve the problems of complicated operation, low intermediate reaction yield, uneconomical reaction, etc., and achieves the effects of high yield and simplified preparation process

Inactive Publication Date: 2018-12-04
GUANGDONG POWER GRID CO LTD +2
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The invention provides a method for preparing methyl heptafluoroisobutyrate, which solves the problem that in the existing method for preparing heptafluoroisobutyronitrile, the raw materials are highly toxic and difficult to obtain, the reaction is a step-by-step reaction, the operation is cumbersome, and the intermediate reaction The technical problem of low yield and uneconomical reaction

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  • Preparation method for methyl heptafluoroisobutyrate

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Embodiment 1

[0036] Under the protection of nitrogen replacement, 12.76g (0.22mol) of potassium fluoride, 19.81g (0.22mol) of dimethyl carbonate, and 100mL of acetonitrile were added in sequence to a 500mL dry autoclave, and slowly filled with 30.00% perfluoropropylene at -70°C. g (0.20mol), react at 70°C for 15h. After the reaction, the valve of the autoclave was opened in an ice-water bath, unreacted perfluoropropene was released slowly, the remaining reaction liquid was simply distilled, and the fraction at 35-37°C was collected to obtain 33.29 g of the product methyl heptafluoroisobutyrate, with a yield of 73.0%.

Embodiment 2

[0038] Under the protection of nitrogen replacement, 9.24g (0.22mol) of sodium fluoride, 19.81g (0.22mol) of dimethyl carbonate, and 100mL of acetonitrile were added sequentially to a 500mL dry autoclave, and slowly filled with 30.00% perfluoropropylene at -70°C g (0.20mol), react at 70°C for 15h. After the reaction was over, open the autoclave valve in the ice-water bath, slowly release the unreacted perfluoropropene, carry out simple distillation on the remaining reaction liquid, collect the fraction at 35-37°C, and obtain the product methyl heptafluoroisobutyrate 33.56g, the yield 73.6%.

Embodiment 3

[0040] Under the protection of nitrogen replacement, 12.76g (0.22mol) of potassium fluoride, 19.81g (0.22mol) of dimethyl carbonate, and 100mL of diethylene glycol dimethyl ether were successively added to a 500mL dry autoclave, and slowly Charge 30.00 g (0.20 mol) of perfluoropropylene, and react at 70° C. for 15 h. After the reaction, the valve of the autoclave was opened in an ice-water bath, unreacted perfluoropropene was released slowly, the remaining reaction liquid was simply distilled, and the fraction at 35-37°C was collected to obtain 29.77 g of the product methyl heptafluoroisobutyrate, with a yield of 65.3%.

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Abstract

The invention relates to the technical field of organic synthesis, and in particular relates to a preparation method for methyl heptafluoroisobutyrate. The preparation method for the methyl heptafluoroisobutyrate disclosed by the invention comprises the following steps: under nitrogen or inert gas replacement protection, performing a reaction on dimethyl carbonate, an alkali metal fluoride and perfluoropropylene to obtain the methyl heptafluoroisobutyrate. According to the method disclosed by the invention, the cheap dimethyl carbonate easy to obtain is adopted to replace strictly-controlled highly-toxic product methyl chloroformate as a raw material for preparing the methyl heptafluoroisobutyrate, a one-pot method is adopted to synthesize the methyl heptafluoroisobutyrate, so that the preparation process is simplified; and in addition, a yield of the methyl heptafluoroisobutyrate prepared by the preparation method can reach up to 73.6%, and the technical problems that in a current preparation method for the methyl heptafluoroisobutyrate, raw materials have high toxicity and are not easy to obtain, a reaction is performed by a multi-step process, operation is cumbersome, an intermediate reaction has a low yield, and the reaction is uneconomical are solved.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a preparation method of methyl heptafluoroisobutyrate. Background technique [0002] Methyl heptafluoroisobutyrate can be used in the synthesis of high-voltage insulating gas heptafluoroisobutyronitrile, and is an important fluorine-containing intermediate. At present, the synthesis of heptafluoroisobutyrates is firstly the reaction of methyl chloroformate with potassium fluoride, followed by post-treatment to obtain methyl fluoroformate, and then the reaction with perfluoropropene to obtain heptafluoroisobutyrate. [0003] Yet above-mentioned reaction has following shortcoming: 1, this reaction raw material methyl chloroformate is highly poisonous, strict control, is difficult for obtaining; 2, single-step yield of methyl fluoroformate is extremely low, and reaction is uneconomical; Step by step, the operation is relatively cumbersome. Contents of the invention [...

Claims

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Application Information

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IPC IPC(8): C07C69/63C07C67/27C07C67/54
CPCC07C67/27C07C67/54C07C69/63
Inventor 唐念吴永明李丽田长青邹庄磊周永言樊小鹏
Owner GUANGDONG POWER GRID CO LTD
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