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Synthesis method of 4, 4'-dihydroxy benzophenone

A technique for the synthesis of dihydroxybenzophenone, which is applied in the direction of condensation to prepare carbonyl compounds and organic chemistry, can solve the problems of large environmental pollution, high cost, and low yield, and achieve environmental friendliness, easy operation, and post-processing simple effect

Inactive Publication Date: 2013-10-09
HEILONGJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The present invention aims to solve the problems of large environmental pollution, high cost and low yield in the existing method for synthesizing 4,4'-dihydroxybenzophenone, and provides a kind of 4,4'-dihydroxybenzophenone synthesis method

Method used

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  • Synthesis method of 4, 4'-dihydroxy benzophenone
  • Synthesis method of 4, 4'-dihydroxy benzophenone
  • Synthesis method of 4, 4'-dihydroxy benzophenone

Examples

Experimental program
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specific Embodiment approach 1

[0021] Embodiment 1: In this embodiment, a method for synthesizing 4,4'-dihydroxybenzophenone is carried out according to the following steps:

[0022] Add p-hydroxybenzoic acid, phenol, acidic catalyst and dehydrating agent to the organic solvent, react at a temperature of 40°C to 100°C for 3h to 15h under stirring conditions, separate the liquid, keep the lower reaction liquid, and then pour the lower reaction liquid Stir in water for 30 minutes to obtain a suspension, filter the obtained suspension to obtain a crude product, and then use a mixed solution of ethanol-water to recrystallize the crude product to obtain 4,4'-dihydroxybenzophenone; Wherein, the molar ratio of the p-hydroxybenzoic acid and phenol is 1:(1~1.5); the molar ratio of the p-hydroxybenzoic acid and the acidic catalyst is 1:(2~8); the dehydrating agent The mass ratio with acidic catalyst is (0~10%): 1; The mass of described acidic catalyst and the volume ratio of organic solvent are (0.5~3) g: 1mL; Descri...

specific Embodiment approach 2

[0031] Embodiment 2: This embodiment differs from Embodiment 1 in that the molar ratio of p-hydroxybenzoic acid to phenol is 1:(1.05-1.2). Others are the same as in the first embodiment.

specific Embodiment approach 3

[0032] Embodiment 3: This embodiment is different from Embodiment 1 or Embodiment 2 in that: the molar ratio of the p-hydroxybenzoic acid to the acidic catalyst is 1:(3-4). Others are the same as in the first or second embodiment.

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Abstract

The invention discloses a synthesis method of 4, 4'-dihydroxy benzophenone, relating to a synthesis method of 4, 4'-dihydroxy benzophenone. The invention aims at solving the problems of great environmental pollution, high cost and low yield of the existing synthesis method of the 4, 4'-dihydroxy benzophenone. According to the method, p-hydroxybenzoic acid and phenol are taken as raw materials, and an acid catalyst and a dehydrating agent are used in an organic solvent to realize one-step high-efficient synthesis of the 4, 4'-dihydroxy benzophenone. The method disclosed by the invention is simple and convenient to operate, the p-hydroxybenzoic acid and the phenol are taken as the raw materials for one-step synthesis of the 4, 4'-dihydroxy benzophenone, and the production cost is reduced; the reaction conditions are mild, and the method is environment-friendly; and the 4, 4'-dihydroxy benzophenone is easy to separate from a reaction mixture after reaction, the post-treatment is simple, the yield is above 90%, compared with the yield of the existing method, which is 49.1%-68%, the yield is improved by 22%-40.9%, and the method is suitable for industrial production. The method disclosed by the invention can be used for synthesizing the 4, 4'-dihydroxy benzophenone.

Description

technical field [0001] The invention relates to a synthesis method of 4,4'-dihydroxybenzophenone. Background technique [0002] 4,4'-Dihydroxybenzophenone (4,4'-Dihydroxybenzophenone) is a very important organic synthesis intermediate, which is widely used in daily chemical industry, photosensitive, pharmaceutical, pesticide, plastic, coating and other fields. Its structural formula is: [0003] [0004] With the increasing demand for pharmaceutical raw materials, photosensitive materials and other products in domestic and foreign markets, the synthesis of 4,4'-dihydroxybenzophenone has received more attention. [0005] There are many reports about its synthesis. Japanese Patent JP3123752 reports that p-hydroxybenzoic acid and phenol are used as raw materials, and polyphosphoric acid is used as solvent to directly catalyze the synthesis of the target compound. However, this method requires a large amount of polyphosphoric acid, which makes it difficult to recycle waste ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/45
Inventor 孙志忠石晓红侯艳君初文毅于微微张婉莹
Owner HEILONGJIANG UNIV