Method for preparing p-chlorodiphenyl ketone

A technology of p-chlorobenzophenone and p-chlorobenzoic acid is applied in the field of preparation of p-chlorobenzophenone, can solve the problems of large amount of catalyst, many three wastes and high yield, and achieves reduction of reaction steps and equipment investment. , to avoid the effect of multi-step reactions

Inactive Publication Date: 2015-05-13
JIANGSU MARINE RESOURCES DEV RES INST LIAN YUNGANG +1
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

The most important preparation method of p-chlorobenzophenone is: (1) Friedel-Crafts acylation reaction method of p-chlorobenzoyl chloride and benzene, this method is simple and easy, and the yield is as high as more than 90%, and the disadvantage is that 1 mol of Chlorobenzoyl chloride needs to use more than 2mol of anhydrous AlCl3 as a catalyst. After the reaction, it must be hydrolyzed with an acidic aqueous solution to obtain p-chlorobenzophenone, which produces a large amount of aluminum-containing salt Waste acid is unfavorable in terms of economic cost and environmental protection
(2) Benzoyl chloride and chlorobenzene are condensed under the catalysis of anhydrous AlCl3 to obtain p-chlorobenzophenone [Journal of Shanxi Un

Method used

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  • Method for preparing p-chlorodiphenyl ketone

Examples

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Effect test

example 1

[0020] 6 moles of benzene, 1.5 moles of p-chlorobenzoic acid, 1.5 moles of p-chlorobenzotrichloride and 0.006 moles of ferric chloride were mixed in a 1-liter pressure reactor. The lid of the reaction kettle was tightened and placed in a hot bath with an electromagnetic stirring speed of 50-150rpm. All valves were closed at the beginning of the reaction, hydrogen chloride gas was released from the gas escape valve and in turn received into the ice bath cooled sodium hydroxide absorbent. Start heating for about 30 minutes and the temperature reaches 160°C. As the temperature increases, the pressure on the reactor increases to 0.5MPa. Open the gas escape valve on the top of the reactor to let the hydrogen chloride gas slowly escape into the sodium hydroxide solution. The pressure is maintained React at 0.75 MPa, the temperature is 175 ° C, after 8 hours of reaction, basically no hydrogen chloride gas escapes, the reaction substance is cooled to room temperature, then the reactio...

example 2

[0022] 5 moles of benzene, 1 mole of p-chlorobenzoic acid, 1 mole of p-chlorotrichlorotoluene and 0.004 moles of zinc chloride were mixed in a 1-liter pressure reactor. The reaction pressure was maintained at 0.7 MPa, the temperature was 165° C., and the reaction was carried out for 6 hours. Other operations were the same as in Example 1. The yield of p-chlorobenzophenone is 89%.

example 3

[0024] 6 moles of benzene, 1.5 moles of p-chlorobenzoic acid, 1.5 moles of p-chlorotrichlorotoluene and 0.005 moles of zinc benzoate were mixed in a 1-liter pressure reactor. Pressure 0.5MPa, temperature 150 ℃, reacted 10 hours, other operations were with example 1, and the yield of p-chlorobenzophenone was 80%.

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Abstract

The invention discloses a method for preparing p-chlorodiphenyl ketone. According to the method, p-chlorotrichloromethyl benzene, p-chlorobenzoic acid and benzene are subjected to Friedel-Crafts reaction in the presence of a catalytic amount of Lewis acid, such as FeCl3 to prepare p-chlorodiphenyl ketone. The method is performed under the conditions of a heating temperature of 150 DEG C-180 DEG C and a pressure of 0.5-0.8MPa, the molar ratio of p-chlorotrichloromethyl benzene to benzene is 1: (2-5), the molar ratio of p-chlorobenzoic acid to p-chlorotrichloromethyl benzene is 1: 1, the yield of p-chlorodiphenyl ketone is 90%, the disadvantage of aluminum-salt-containing wastewater pollution caused by catalysis of equimolar anhydrous AlCl3 used in the conventional acylation method is eliminated, the multi-step reaction of firstly preparing acyl chloride and then carrying out acylation in the traditional method is avoided, no isomer is generated and the product is high in quality.

Description

technical field [0001] The invention relates to a preparation method of p-chlorobenzophenone, which belongs to the field of chemical preparation. Background technique [0002] 4-Chlorobenzophenone is an important intermediate in organic synthesis, used as a photoinitiator and ultraviolet absorber, and can be used to make UV-curable coatings and inks. It is often used in the preparation of p-chlorobenzhydrylamine in the pharmaceutical industry, which is an important intermediate for the synthesis of levocetirizine for the treatment of allergic diseases. Because the chlorine atom on the p-chlorobenzophenone molecule is affected by the carbonyl group, it is easy to react with nucleophiles, and they are all raw materials for the manufacture of drugs and pesticides. The most important preparation method of p-chlorobenzophenone is: (1) Friedel-Crafts acylation reaction method of p-chlorobenzoyl chloride and benzene, this method is simple and easy, and the yield is as high as more...

Claims

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Application Information

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IPC IPC(8): C07C49/813C07C45/46
CPCC07C45/46
Inventor 张珍明李树安尹福军沙鸥王璇王润南
Owner JIANGSU MARINE RESOURCES DEV RES INST LIAN YUNGANG
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