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The preparation method of 1,1,1-trifluoroacetone

A technology of trifluoroacetate and molar ratio, applied in the preparation of organic compounds, preparation of carbon-based compounds, chemical instruments and methods, etc., can solve the problems of harsh reaction conditions, large pollution, low yield, etc., and achieve low cost , Simple operation, convenient purification effect

Active Publication Date: 2021-11-19
赵博佑
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] In order to solve the current preparation of TFK has harsh reaction conditions, high temperature and high pressure is required, or the raw materials are not easy to obtain, the yield is not high, or the pollution is large, and the purification is difficult. At the same time, the production cost of the product is reduced, and the market competitiveness of the product is improved. The present invention provides A method for preparing TFK by Grignard reaction

Method used

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  • The preparation method of 1,1,1-trifluoroacetone
  • The preparation method of 1,1,1-trifluoroacetone

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Experimental program
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Effect test

Embodiment 1

[0021] In a dry four-neck flask (equipped with a rectification column), under the protection of nitrogen, add 900mL (1.8mol) of 2mol / L tetrahydrofuran solution of methylmagnesium chloride, stir, add 11.4g (0.075mol) of cesium fluoride, and cool down to - A mixed solution of 213.1 g (1.5 mol) of ethyl trifluoroacetate and 375 mL of tetrahydrofuran was added dropwise at 5°C. After dropping, slowly rise to 30°C for 1 hour reaction. Below 10°C, adjust the pH to 1 with 20% hydrochloric acid. Slowly raise the temperature, distill under normal pressure directly, and collect the fraction at 22°C~23°C in a cold trap at -40°C to obtain 153.7g of colorless liquid, namely TFK, with a GC purity of 99.5% (area normalization method) and a yield of 91.5%.

Embodiment 2

[0023] With the technological operation step of embodiment 1, different conditions are:

[0024] Add 1800mL (1.8mol) of tetrahydrofuran solution of 1mol / L methylmagnesium chloride, 4.4g (0.075mol) of potassium fluoride, drop it up to 20°C for 6 hours, and obtain 140.7g of colorless liquid, namely TFK, with a GC purity of 99.2%. Yield 83.7%.

Embodiment 3

[0026] With the technological operation step of embodiment 1, different conditions are:

[0027] Add 600 mL (1.8 mol) of 3 mol / L tetrahydrofuran solution of methylmagnesium chloride, 3.2 g (0.075 mol) of sodium fluoride, drop it up to 30 ° C for 4 hours, and obtain 142.9 g of a colorless liquid, namely TFK, with a GC purity of 99.1%. Yield 85.0%.

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Abstract

The invention discloses a preparation method of 1,1,1-trifluoroacetone. Using methylmagnesium halide Grignard reagent and trifluoroacetate as raw materials, Grignard reaction occurs in ether solvent, followed by acidification and direct distillation to obtain 1,1,1-trifluoroacetone. The method has the advantages of readily available raw materials, convenient post-treatment purification, simple operation, relatively low cost, high yield, and high product purity. The prepared 1,1,1-trifluoroacetone is an important trifluoromethyl synthesis building block and an important organic intermediate for the synthesis of many fluorine-containing medicines, pesticides and polymer materials.

Description

technical field [0001] The invention relates to a preparation method of 1,1,1-trifluoroacetone. Background technique [0002] In recent years, fluorine-containing fine chemicals have attracted the attention of academic and industrial circles at home and abroad. 1,1,1-Trifluoroacetone (TFK) is an important fluorine-containing fine chemical, because it contains CF 3 The special group has many unique and excellent properties, and is an important organic intermediate for the synthesis of many fluorine-containing medicines, pesticides and polymer materials, and is widely used. Trifluoromethyl is difficult to obtain by direct fluorination, and 1,1,1-trifluoroacetone is an important building block for trifluoromethyl synthesis. [0003] The preparation methods reported in the literature include oxidation, reduction, and decarboxylation. In US6340776 and US0034254, it is reported that chlorotrifluoroacetone is used as a raw material, and TFK is prepared through high-pressure hydr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/167C07C45/67C07C45/78
Inventor 赵爱明倪秋洋赵博佑
Owner 赵博佑
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