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2,5-dimethoxy ethyl phenyl sulfide and synthesis method and use thereof

A technology of dimethoxythiophenol and dimethoxybenzene, which is applied to the preparation of sulfides and organic chemistry, and can solve the problems that the synthesis method has not been reported in the literature.

Inactive Publication Date: 2003-08-06
WUHAN UNIV
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Problems solved by technology

[0002] As a new compound, 2,5-dimethoxyphenethyl sulfide and its synthetic method have not been reported in the literature

Method used

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  • 2,5-dimethoxy ethyl phenyl sulfide and synthesis method and use thereof

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Embodiment Construction

[0009] Add 105ml of dichloroethane and 13.5g of p-xylylene dimethyl ether into a 250ml three-necked flask, stir to dissolve, cool in an ice bath (0-10°C), add 26.5ml of chlorosulfonic acid and 10ml of thionyl chloride dropwise under stirring, and react After 2 hours, it was poured into 280ml of ice water under stirring, and the lower oil layer was separated, dichloromethane (recovery) was evaporated, and the yellow solid 2,5-dimethoxybenzenesulfonyl chloride was dried and weighed 19.8g. 85%, melting point 115-117°C.

[0010] Add 68ml of water and 23ml of concentrated sulfuric acid into a 500ml three-necked flask, and when the temperature drops to about 70°C, add 12g of 2,5-dimethoxybenzenesulfonyl chloride and 18g of zinc powder, react at 80°C for 1 hour, filter, Under reduced pressure and distillation, 8.2 g of 2,5-dimethoxythiophenol was obtained.

[0011] Add 3g of potassium hydroxide and 50ml of absolute ethanol into a 250ml three-necked flask, stir to dissolve, add a sol...

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Abstract

The present invention relates to 2,5-dimethoxyethyl phenyl sulfide and its synthesis method. Said invention provides its structure formula, and uses 2,5-dimethoxybenzenesulfonyl chloride as raw material, and adopts the following steps: using zinc powder to make reduction under the acid condition at 70-80 deg.c, then reduced pressure distilling to obtain 2,5-dimethoxythiophenol, making the obtained 2,5-dimethoxthiophenol implement condensation reaction with bromoethane under the alkaline condition at 70-80 deg.C, reduced pressure distilling to obtain the yellow oil liquor, i.e. the required 2,5-dimethoxyethyl phenyl sulfide. It can be used for synthesizing 2,5-dimethoxy-4-ethylthiobenzaldehyde.

Description

technical field [0001] The invention relates to a kind of 2,5-dimethoxyphenethyl sulfide and its synthesis method and application. Background technique [0002] As a new compound, 2,5-dimethoxyphenethyl sulfide and its synthesis method have not been reported in the literature. Contents of the invention [0003] The task of the present invention is to provide a kind of novel compound 2,5-dimethoxyphenethyl sulfide and its synthetic method and application. [0004] The technical scheme provided by the invention is: 2,5-dimethoxyphenethyl sulfide, its structural formula is [0005] The present invention also provides a synthesis method of the above-mentioned compound, using 2,5-dimethoxybenzenesulfonyl chloride as a raw material, reducing with zinc powder at 70-80°C and acidic conditions (pH<1), and then distilling under reduced pressure , to obtain 2,5-dimethoxythiophenol; the resulting 2,5-dimethoxythiophenol is condensed with bromoethane under alkaline conditions (p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/14C07C323/20
Inventor 张治民廖俊张淑娴
Owner WUHAN UNIV