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Method for preparing 4-dichlorodiphenylmethane

A technology of chlorobisphenyl chloride and chlorobenzophenone, which is applied in the field of preparing 4-chlorobisphenyl chloride, can solve the problems of easy combustion of hydrogen, cumbersome treatment process, high reaction temperature, etc., and achieve sufficient reaction and simple process , the effect of low reaction temperature

Inactive Publication Date: 2014-07-02
PEKING UNIV FOUNDER GRP CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses zinc powder as a reducing agent. Zinc powder generally needs to be activated and has strong reducibility. It will release hydrogen gas when it reacts with acid and alkali, and hydrogen gas is very easy to burn and explode.
Therefore, the reaction temperature of this method is high, and it is easy to burn and explode when it encounters air; the reaction time is long, and the processing process is relatively cumbersome; and because benzene is used for extraction, it is highly toxic

Method used

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  • Method for preparing 4-dichlorodiphenylmethane
  • Method for preparing 4-dichlorodiphenylmethane
  • Method for preparing 4-dichlorodiphenylmethane

Examples

Experimental program
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Effect test

Embodiment 1

[0059] Example 1: Add 350ml of absolute ethanol to a three-necked reaction flask, then add 150g of 4-chlorobenzophenone and 12g of potassium borohydride, stir and heat up, and react at about 80°C for 4 hours. After the reaction, the ethanol was distilled to obtain 4-chlorobenzhydryl alcohol. Then, 750 ml of 36% by mass hydrochloric acid aqueous solution was added and stirred to carry out chlorination reaction, and the reaction was carried out at about 77° C. for 4.5 hours. The reaction solution was cooled, and the organic layer was separated to obtain 147.8 g of 4-chlorodiphenylchloromethane. The conversion rate is 90%, and the content is 99.5%.

Embodiment 2

[0060] Example 2: Add 350ml of absolute ethanol to a three-necked reaction flask, then add 150g of 4-chlorobenzophenone and 22.5g of potassium borohydride, stir and heat up, and react at about 70°C for 3.5 hours. After the reaction, the ethanol was distilled to obtain 4-chlorobenzhydryl alcohol. Then, 700 ml of 36% by mass hydrochloric acid aqueous solution was added and stirred to carry out chlorination reaction, and the reaction was carried out at about 80° C. for 4 hours. The reaction solution was cooled, and the organic layer was separated to obtain 149.5 g of 4-chlorodiphenylchloromethane. The conversion rate is 91%, and the content is 99.7%.

Embodiment 3

[0061] Example 3: Add 350ml of absolute ethanol to a three-necked reaction flask, then add 150g of 4-chlorobenzophenone and 15g of potassium borohydride, stir and heat up, and react at about 77°C for 4.5 hours. After the reaction, the ethanol was distilled to obtain 4-chlorobenzhydryl alcohol. Then, 680 ml of 37% by mass hydrochloric acid aqueous solution was added and stirred for chlorination reaction, and the reaction was carried out at about 78° C. for 4.5 hours. The reaction solution was cooled, and the organic layer was separated to obtain 149.6 g of 4-chlorodiphenylchloromethane. The conversion rate is 91%, and the content is 99.5%.

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Abstract

The invention provides a method for preparing 4-dichlorodiphenylmethane. The method comprises the following steps: (1) performing a reduction reaction between 4-chlorobenzophenone and potassium borohydride or sodium borohydride to obtain 4-chlorobenzhydrol; and (2) performing a chlorination reaction between 4-chlorobenzhydrol and a hydrochloric acid aqueous solution to prepare the 4-dichlorodiphenylmethane. The method can be used for improving the conversion rate and purity of a product, is simple in process, is safe and stable because no gas is generated in the reacting process, is low in cost, and has an extremely high practical value in the industry.

Description

technical field [0001] The invention belongs to the field of pharmacy, and in particular relates to a method for preparing 4-chlorobisphenylchloromethane. Background technique [0002] The molecular formula of 4-chlorobisphenylchloromethane (English name: 4-Chlobenzhydryl Chloride) is: C 13 h 10 Cl 2 , the molecular weight is 237.13, the CAS number is 134-83-8, and its structural formula is: [0003] [0004] 4-Chlorodiphenylchloromethane is a reactant for the synthesis of meclizine or meclizine hydrochloride. Meclizine hydrochloride is suitable for various skin and mucous membrane allergic diseases, and can also be used for nausea and vomiting caused by pregnancy, radiotherapy and motion sickness. It is an antagonist of histamine receptors, and its effect is far longer than diphenhydramine. Stays for 12-24 hours. [0005] The method for the preparation of 4-chlorobisphenylchloromethane reported at present is seldom, and generally known method is: add 4-chlorobenzoph...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C25/18C07C17/16
Inventor 王启丽赵德李明川杨通明
Owner PEKING UNIV FOUNDER GRP CO LTD
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