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2,5-dimethoxy-4-ethyl sulfide-beta-nitrostyrolene and preparation process and use thereof

A kind of technology of nitrostyrene and dimethoxy thiophenol, applied in 2 fields

Inactive Publication Date: 2003-08-06
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] As a new compound, 2,5-dimethoxy-4-ethylthio-β-nitrostyrene and its synthetic method have not been reported in the literature

Method used

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  • 2,5-dimethoxy-4-ethyl sulfide-beta-nitrostyrolene and preparation process and use thereof

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Experimental program
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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, and dichloromethane (recovery) was evaporated to obtain yellow solid 2,5-dimethoxybenzenesulfonyl chloride, with a dry weight of 19.8g and a yield of 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 ...

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Abstract

The present invention relates to 2,5-dimethoxy-4-ethylthio-beta-nito-styrene and its method for preparing the above-mentioned compound. 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 reductino under the acidic condition at 70-80 deg.C, reduced pressure distilling to obtain 2,5-dimethoxythiophenol, making it and bromoethane undergo the process of condensation reaction under the alkaline condition at 70-80 deg.C, reduced pressure distilling to obtain 2.5-dimethoxyethyl phenylsulfide, making it and phosphorus oxychloride and dimethyl formamide produce reaction at 70-80 deg.C to obtain 2,5-dimethoxy-4-ethylthiobenzaldehyde.

Description

technical field [0001] The present invention relates to 2,5-dimethoxy-4-ethylthio-β-nitrostyrene and its preparation method and application. Background technique [0002] As a new compound, 2,5-dimethoxy-4-ethylthio-β-nitrostyrene 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 new compound 2,5-dimethoxy-4-ethylthio-β-nitrostyrene and its preparation method and application. [0004] The technical scheme provided by the present invention is: 2,5-dimethoxy-4-ethylthio-β-nitrostyrene, whose structural formula is [0005] The present invention also provides a method for preparing the above-mentioned compound, using 2,5-dimethoxybenzenesulfonyl chloride as a raw material, reducing it with zinc powder at 70-80°C and acidic conditions (pH<1), and then distilling it under reduced pressure , to obtain 2,5-dimethoxythiophenol; the resulting 2,5-dimethoxythiophenol is conden...

Claims

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Application Information

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