Preparation method of 4,4'-dihydroxydiphenyl ether

A technology of dihydroxydiphenyl ether and dichloroethane, which is applied in the field of pharmaceutical intermediates and pesticides, can solve the problems of high safety protection and environmental monitoring, unsuitable for industrial production needs, strong irritation and corrosiveness, and achieve reaction The effect of short process route, low raw material price and easy product

Inactive Publication Date: 2014-04-16
STONE LAKE PHARMA TECH
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Problems solved by technology

However, a large amount of bromine needs to be used in this method. Because bromine is toxic, highly irritating and corrosive, it has high requirements for industrial equipment, safety protection and environmental monitoring, and does not meet the national green and environmental protection production indicators, so it is not suitable for future use. Long-term industrial production needs

Method used

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  • Preparation method of 4,4'-dihydroxydiphenyl ether
  • Preparation method of 4,4'-dihydroxydiphenyl ether

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Embodiment Construction

[0023] The present invention will be described in detail below in conjunction with embodiments.

[0024] A kind of preparation method of 4,4'-dihydroxy diphenyl ether, it is characterized in that, the method comprises the following steps:

[0025] Step 1) Under the protection of nitrogen, add 20.4g of acetyl chloride, 33.3g of aluminum trichloride and 80mL of dichloroethane into the flask, then add dropwise a solution of 14.3g of diphenyl ether in dichloroethane (20mL) while stirring, The dropping temperature was controlled at 50°C. After the dropping was completed, the temperature was maintained to continue heating and stirring, followed by TLC spotting. After the reaction, cool down to room temperature, pour it into ice water to quench the reaction, and then extract with ethyl acetate (100 mL×3), combine the organic phases, wash with dilute hydrochloric acid and saturated brine, and wash with anhydrous Na 2 SO 4 dry. After filtration, the solvent was removed in vacuo to o...

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Abstract

The invention discloses a preparation method of 4,4'-dihydroxydiphenyl ether. The preparation method comprises the following steps that diphenyl ether undergoes a Friedel-Crafts acylation reaction to produce 4,4'-diacetyldiphenyl ether; and the 4,4'-diacetyldiphenyl ether is synthesized into 4,4'-dihydroxydiphenyl ether under the action of a hydrogen peroxide aqueous solution having the content of 30%, boric acid and a catalytic amount of an acid. The preparation method has the advantages of low raw material price, short reaction technology route, high reaction yield and easy separation of products.

Description

technical field [0001] The invention relates to pesticides and pharmaceutical intermediates, in particular to a preparation method of 4,4'-dihydroxydiphenyl ether. Background technique [0002] Studies have confirmed that 4,4'-dihydroxydiphenyl ether compounds are a very important class of intermediates, which are widely used in the fields of pesticides, medicines, spices, plastics and liquid crystal materials. [0003] The research on the preparation method of 4,4'-dihydroxydiphenyl ether compounds in the published literature reports mainly contains the following aspects: [0004] As early as 1931, Oesterlin et al. reported in Monatshefte fuer Chemie a method for preparing 4,4'-dihydroxydiphenyl ether from 4-methoxybromobenzene, but this synthetic route required high temperature heating, and the synthetic yield Low (minimum to 41%), etc., not suitable for industrial mass production. [0005] [0006] In 1932, Chem. Fabr. v. Heyden reported in the patent DE609080 that 4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/295C07C41/26
CPCC07C41/26C07C45/46C07C43/295C07C49/84
Inventor 吕少波
Owner STONE LAKE PHARMA TECH
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