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A kind of preparation method of benzophenone compound

A technology for diphenylmethane and benzophenone, applied in the field of oxidative preparation of benzophenone, can solve the problems of difficulty in compliance with environmental protection regulations, low catalyst stability, low catalyst activity, etc., and achieves less demanding equipment requirements and post-treatment. Convenient, responsive and simple to operate

Active Publication Date: 2021-02-09
TIANJIN JIURI NEW MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although great progress has been made in the research on catalysts for the preparation of benzophenone compounds, there are still problems in these processes, such as low catalyst activity, cumbersome preparation process, or the need for strong oxidants and by-products.
In addition, problems such as low stability of the catalyst also limit its use.
Moreover, it is difficult for metal-containing catalysts (especially heavy metal-containing catalysts) to meet the increasingly stringent environmental regulations.

Method used

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  • A kind of preparation method of benzophenone compound

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: the preparation method of benzophenone

[0031] Diphenylmethane (33.6g, 0.2mol), TEMPO (1.6g, 0.01mol) and KBr (7.1g, 0.06mol) were dissolved in 100mL of dichloroethane, after stirring evenly, 30% hydrogen peroxide (68.0 g, 0.6mol), after 30 minutes of dripping, then stirred for the reaction, and the reaction was monitored by TLC. After the reaction, saturated sodium thiosulfate solution was added dropwise to carry out the extraction reaction. The organic phase was separated, washed with water, and dried. First, the solvent was recovered by distillation, and then the product benzophenone was purified by vacuum distillation. 31.0 g of 110-118 °C / 1 Torr fraction were collected, with a purity of 99.4% and a yield of 85%.

Embodiment 2

[0032] Embodiment 2: the preparation method of benzophenone

[0033] Diphenylmethane (33.6g, 0.2mol), TEMPO (1.6g, 0.01mol) and KBr (7.1g, 0.06mol) were dissolved in 100mL of acetonitrile, after stirring evenly, 30% hydrogen peroxide (68.0g, 0.6 mol), after 30 minutes of dripping, then stirred and reacted, and the reaction was monitored by TLC. After the reaction, saturated sodium thiosulfate solution was added dropwise to carry out the extraction reaction. , separated the organic phase, washed with water, dried, distilled to recover dichloromethane first, then purified the product benzophenone by vacuum distillation, collected 110~118°C / 1 Torr fraction 31.0g, the purity was 99.6%, and the yield was 83%.

Embodiment 3

[0034] Embodiment 3: the preparation method of benzophenone

[0035] Diphenylmethane (33.6g, 0.2mol), TEMPO (1.6g, 0.01mol) and KBr (7.1g, 0.06mol) were dissolved in 100mL of dichloroethane, after stirring evenly, 30% hydrogen peroxide (68.0 g, 0.6mol), after 30 minutes of dripping, then stirred for the reaction, and the reaction was monitored by TLC. After the reaction, saturated sodium thiosulfate solution was added dropwise to carry out the extraction reaction. The organic phase was separated, washed with water, and dried. First, the solvent was recovered by distillation, and then the product benzophenone was purified by vacuum distillation. 31.0 g of 110-118 °C / 1 Torr fraction were collected, with a purity of 99.4% and a yield of 85%.

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Abstract

The preparation method of benzophenone provided by the invention is to use diphenylmethane as a raw material, and under the action of a catalyst, add oxidant H 2 o 2 Oxidation is carried out to obtain diphenyl ketone. The method has the advantages of using an environmentally friendly oxidant, mild reaction conditions, simple and convenient operation; the product does not contain heavy metals or transition metal ions; less side reactions, high reaction yield; high safety, no strict requirements on equipment, easy operation, and suitable for industrial production Etc.

Description

technical field [0001] The invention relates to a method for preparing a compound benzophenone, in particular to a method for preparing benzophenone by oxidation using diphenylmethane as a raw material. Background technique [0002] Benzophenone is a very important fine chemical, which is a colorless crystal at normal temperature and pressure. It is mainly used in the synthesis of drugs, the manufacture of fragrances, and can also be used in film manufacturing. Benzophenone compounds are widely used in pharmaceutical synthesis, fragrance industry and polymer materials, and can also be used in photocuring industry as photoinitiators. [0003] At present, the industrial synthesis routes of benzophenone compounds mainly include carbonylation, acylation, and nitric acid oxidation. The carbonylation method generally reacts under high temperature and high pressure; a large amount of waste acid is generated during the acylation method, which corrodes the equipment and makes it dif...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/28C07C49/786C07C49/784C07C49/813
CPCC07C45/28C07C49/786C07C49/784C07C49/813
Inventor 吴彬罗想武瑞任凤霞张建锋张齐
Owner TIANJIN JIURI NEW MATERIALS CO LTD