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Phenol analog derivative preparation method

A technology of derivatives and phenols, which is applied in the field of preparation of phenol derivatives, can solve the problems of high ammonium persulfate dosage, harsh operating conditions, and high dosage of glacial acetic acid in the feeding method, so as to achieve high production efficiency, reduce dosage and concentration, The effect of large feeding coefficient

Active Publication Date: 2007-08-01
烟台九目化学股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method avoids the shortcoming that previous literature prepares phenol benzene derivative to a certain extent, also exists the unavoidable shortcoming of industrial production: (1) feeding method and ammonium persulfate consumption are too high, poor safety in production, difficult to operate The conditions are harsh; (2) the dosage of glacial acetic acid is too high, which determines that its feed coefficient is very low, thereby the production efficiency is low and the production cost is high; more importantly, the use of a large amount of glacial acetic acid in industry will inevitably cause harm to the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 preparation of

[0028] Add 274.4 grams (15.2mol) of water and 117.6 grams (1.2mol) of concentrated sulfuric acid in the two liters of reaction flask, prepare the dilute sulfuric acid solution of 30% mass concentration, with 345 grams (1.5mol) (GC: 94%), 447 grams (7.5 mol) of glacial acetic acid, and 69 ml of toluene were added to the reaction flask, stirred and cooled to 20°C, and 410.4 grams (1.8 mol) of ammonium persulfate was slowly added. Then keep it warm at 20-70°C for 20 hours. Add 500ml (500 grams) of water to the system, stir for 20 minutes, filter, filter cake with water until neutral, and dry to obtain 305 grams of crude product. GC purity 94.2%, yield 99.7%.

Embodiment 2

[0029] Example 2 preparation of

[0030] Add 243 grams (15.2mol) of water and 117.6 grams (1.2mol) of concentrated sulfuric acid in the two liters of reaction flask, the dilute sulfuric acid solution of the mass concentration of preparation 20%, with 408 grams (1.5mol) (GC: 92.6%), 447 grams (7.5 mol) of glacial acetic acid, and 69 ml of dichloromethane were added to the reaction flask, stirred and cooled to 25° C., and 410.4 grams (1.8 mol) of trifluoroperacetic acid was slowly added. Then keep it warm at 20-70°C for 10 hours. Add 500ml (500 grams) of water to the system, stir for 20 minutes, filter, filter cake with water until neutral, and dry to obtain 367 grams of crude product. GC purity 96.7%, yield 99.4%.

Embodiment 3

[0031] Example 3 preparation of

[0032] Add 273.6 grams (15.2mol) of water and 117.6 grams (1.2mol) of concentrated sulfuric acid in the two liters of reaction flask, prepare the dilute sulfuric acid solution of 40% mass concentration, with 357 grams (1.5mol) (GC: 97.1%), 447 grams (7.5 mol) of glacial acetic acid, and 71.4 ml of methanol were added to the reaction flask, stirred and cooled to 20° C., and 486 grams (1.8 mol) of potassium persulfate was slowly added. Then keep it warm at 20-70° C. for 5 hours, add 500 ml (500 grams) of water to the system, stir for 20 minutes, filter, pour the filter cake with water until neutral, and dry to obtain 305 grams of crude product. GC: 95.8%, yield 95.9%.

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Abstract

The invention discloses a making method of phenol derivant, which comprises the following steps: (1) adopting acetophenone derivant as raw material and dilute sulfuric acid as catalyst; adding raw material, catalyst, glacial acetic acid and organic solvent into reacting container; (2) stirring; adding oxidizer into the system slowly; (3) insulating at 10-70 deg.c for 5-20h.

Description

1. Technical field [0001] The invention relates to a preparation method of phenol derivatives, belonging to the technical field of preparation of phenol derivatives. 2. Background technology [0002] Phenol derivatives are an important class of intermediates for the industrial preparation of liquid crystals and medicines. [0003] U.S. Patent No. 3,992,459 discloses a method for preparing 4-(2,4-difluorophenyl)phenol, which first oxidizes 4-(2,4-difluorophenyl)acetophenone to 4-(2,4- Difluorophenyl) phenol acetate, after hydrolysis, it is processed into 4-(2,4-difluorophenyl) phenol; The preparation method of (cyclohexyl) phenol, its principle and method are similar with above-mentioned U.S. patent; Above-mentioned two kinds of methods are divided into two-step reaction, comparatively complicated, are unfavorable for industrial production. [0004] German Merk company patent DE2636684 introduces a kind of preparation method of 4-(4-alkylcyclohexyl)phenol: in oxidant H 2 o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C37/56C07C37/00
Inventor 宋有永王大鹏崔阳林陈敬军
Owner 烟台九目化学股份有限公司
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