Method for synthesizing 2,3,4,4'-tetrahydroxybenzophenone

A technology of tetrahydroxybenzophenone and p-hydroxybenzoic acid, which is applied in the direction of chemical instruments and methods, condensation preparation of carbonyl compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of large amount of waste liquid, reaction Long time and other problems, to achieve the effect of short reaction time, reduce preparation cost, and reduce the amount of waste liquid

Inactive Publication Date: 2010-09-01
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction conditions of this method are mild, but the reaction time is long and the amount of waste liquid produced is large

Method used

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  • Method for synthesizing 2,3,4,4'-tetrahydroxybenzophenone
  • Method for synthesizing 2,3,4,4'-tetrahydroxybenzophenone
  • Method for synthesizing 2,3,4,4'-tetrahydroxybenzophenone

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Embodiment 1

[0023] A process for synthesizing 2,3,4,4'-tetrahydroxybenzophenone, the steps are:

[0024] (1) According to the mass ratio of pyrogallic acid and p-hydroxybenzoic acid as 1: 1.1 (mol: mol), pyrogallic acid and p-hydroxybenzoic acid are acylated under a certain catalyst and temperature, and the reaction ends After cooling, the reaction solution was neutralized with alkaline solution to precipitate crystals, filtered, washed with water and dried to obtain a crude product of 2,3,4,4'-tetrahydroxybenzophenone. The catalyst used in the acylation reaction is boron trifluoride methanol solution, the ratio of the amount to the quality of pyrogallic acid is 4:1 (mL:g); the lye is 3-5% (g / mL) sodium bicarbonate solution , the amount of lye used is to control the pH value of the solution to a neutral limit; the reaction temperature is 100-120°C; the reaction time is 2-6h.

[0025] (2) Dissolve the crude product of 2,3,4,4'-tetrahydroxybenzophenone obtained by the reaction in boiling w...

Embodiment 2

[0027] (1) Weigh 6.3g of pyrogallic acid and 7.6g of p-hydroxybenzoic acid, put them into a 500mL three-necked reaction flask, add 25mL of methanol solution of boron trifluoride as a catalyst, and react at 110°C for 6h, cool after the reaction, and the reaction solution Neutralize with 3% (g / mL) sodium bicarbonate solution, adjust the pH value to neutral, precipitate crystals, filter, wash with water and dry to obtain the crude product of 2,3,4,4'-tetrahydroxybenzophenone 10.06 g.

[0028] (2) The above crude product was dissolved in 500mL of boiling water, added 1.5g of activated carbon for decolorization for 20min, filtered while hot, the filtrate was cooled and crystallized, filtered, washed with pure water, dried to obtain 2,3,4,4'-tetrahydroxybenzidine Ketone refined product 7.72g.

Embodiment 3

[0030] Weigh 6.3g of pyrogallic acid and 7.6g of p-hydroxybenzoic acid, put them into a 500mL three-necked reaction flask, add 25mL of methanol solution of boron trifluoride as catalyst, react at 120°C for 2h, cool after the reaction, and use 5% (g / mL) sodium bicarbonate solution to neutralize, adjust the pH value to neutral, precipitate crystals, filter, wash with water and dry to obtain 9.1 g of crude product of 2,3,4,4'-tetrahydroxybenzophenone.

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Abstract

The invention relates to a method for synthesizing 2,3,4,4'-tetrahydroxybenzophenone. In the method, methanol solution of boron trifluoride is used as a catalyst, pyrogallic acid and p-hydroxybenzoic acid are used as the raw materials to synthesize the 2,3,4,4'-tetrahydroxybenzophenone. The method is characterized in that: the methanol solution of boron trifluoride is used as a catalyst; and the pyrogallic acid and the p-hydroxybenzoic acid undergo an acylation reaction at a certain temperature to form the 2,3,4,4'-tetrahydroxybenzophenone.

Description

technical field [0001] The invention relates to a process for synthesizing 2,3,4,4'-tetrahydroxybenzophenone: using boron trifluoride as a catalyst, pyrogallic acid and p-hydroxybenzoic acid as raw materials to synthesize 2,3, 4,4'-Tetrahydroxybenzophenone. Background technique [0002] 2,3,4,4'-Tetrahydroxybenzophenone (THBP) is an important organic intermediate, which can be used in photoresists, pharmaceutical intermediates, ultraviolet absorbers, resins in the microelectronics integrated circuit industry Stabilizers, dyes, etc. Especially in today's rapid development of the microelectronics industry, the demand for THBP used as an intermediate of UV positive photoresist photoresist increases sharply. my country is one of the main producers of the integrated circuit industry in the world. The output of large-scale integrated circuits accounts for more than 1 / 6 of the global output. The application fields and scope of products are expanding rapidly. At present, research...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/46B01J31/22
Inventor 张亮亮汪咏梅陈笳鸿吴冬梅徐曼吴在嵩汤先赤陈学勇张全
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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