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Method for preparing 3,3'-bis (trifluoromethyl) benzophenone

A technology of trifluoromethyl and benzophenone, applied in 3 fields, can solve the problems of difficult industrialization of Grignard reaction, and achieve the effects of easy industrialization, low production cost and easy operation

Active Publication Date: 2013-05-22
SHANGHAI HETENG FINE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Document Bull.Soc.Chim.France 1962,587-93 mentions the preparation of 3,3`-di (Trifluoromethyl)benzophenone, but the Grignard reaction is difficult to industrialize

Method used

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  • Method for preparing 3,3'-bis (trifluoromethyl) benzophenone
  • Method for preparing 3,3'-bis (trifluoromethyl) benzophenone

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Mix 10 grams of raw material 3,3'-bis(trifluoromethyl)benzenemethane, 100 grams of solvent chloroform and 0.2 gram of catalyst phosphorus pentachloride, then under the illumination of 100w incandescent light and reflux at 60°C, pass 7 grams in 20 hours Chlorine gas, the reaction process was followed by GC and NMR;

[0024] After the reaction is completed, cool, add water, extract with chloroform, separate layers, and after the oil layer is concentrated, the intermediate colorless oily substance 3,3'-bis(trifluoromethyl)phenyldichloromethane is obtained;

[0025] The intermediate 3,3`-bis(trifluoromethyl)phenyldichloromethane, 30 grams of water, 12 grams of acetonitrile and 3 grams of sodium hydroxide were mixed and refluxed for 4 hours, cooled and filtered to obtain the crude product, which was recrystallized with ethanol to obtain 7.8 g of the target product as white crystals, 3,3'-bis(trifluoromethyl)benzophenone, melting point: 102-104°C.

[0026] The yield of the a...

Embodiment 2

[0028] 10 grams of raw material 3,3'-bis(trifluoromethyl)benzene methane, 200 grams of solvent carbon tetrachloride and 0.3 gram of catalyst phosphorus pentachloride were mixed, then under the illumination of 100w incandescent lamp, 12 hours under reflux at 80 DEG C 9.5 grams of chlorine gas, the reaction process was followed by GC and NMR; the reaction was completed, cooled, added water, extracted with carbon tetrachloride, layered, and the oil layer was concentrated to obtain the intermediate colorless oil 3,3`-bis(trifluoromethyl ) phenyl dichloromethane.

[0029] The intermediate 3,3`-bis(trifluoromethyl)phenyldichloromethane mixed with 50 grams of water, 15 grams of acetonitrile and 5 grams of potassium hydroxide was refluxed for 4 hours, cooled and filtered to obtain the crude product, which was recrystallized with ethanol to obtain 8.9 g of the white crystalline target product 3,3'-bis(trifluoromethyl)benzophenone, melting point: 102-104 degrees. The yield of the above...

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PUM

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Abstract

The invention provides a method for preparing 3,3'-bis (trifluoromethyl) benzophenone, which comprises the following steps of: irradiating 3,3'-bis (trifluoromethyl) diphenylmethane used as a raw material with light of a filament lamp for carrying out chlorination reaction; and then carrying out basic hydrolysis to obtain the 3,3'-bis (trifluoromethyl) benzophenone. The invention has the advantages of simple and convenient operation method and low production cost and is convenient to industrialization. The reaction formula is described as below.

Description

technical field [0001] The present invention relates to the preparation method of 3,3'-bis(trifluoromethyl)benzophenone. Background technique [0002] 3,3`-bis(trifluoromethyl)benzophenone is a kind of ultraviolet absorber, also is a kind of medicine, pesticide chemical intermediate, has very extensive application in fields such as medicine, pesticide; In addition, can also be used in Synthesis of fluoropolymer materials. At present, there are mainly the following preparation methods: [0003] Document DE3411326, EP0156278 mentions to take 3,3 '-bis (trifluoromethyl) phenylmethane as raw material and obtain target product 3 with 65% nitric acid reflux, 3 '-bis (trifluoromethyl) benzophenone, productive rate is about 65%, and a large amount of waste acid will be produced at the same time. [0004] Document Bull.Soc.Chim.France 1962,587-93 mentions the preparation of 3,3`-di (Trifluoromethyl)benzophenone, but the Grignard reaction is difficult to industrialize. Contents ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C49/813C07C45/43
Inventor 施冠成滑国钰蔡烨锋夏伟冬
Owner SHANGHAI HETENG FINE CHEM
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