反应详情

To 20 g of crushed ice were added 3.7 ml of concentrated sulfuric acid and 1.90 g of 5-chlorosulfonyl-2,4-dimethoxybenzoic acid. Under ice-cooling, 2.40 g of zinc powder was added, and the mixture was then heated under reflux. After completion of the reaction, the reaction solution was diluted with ethyl acetate and insoluble matter was removed by celite filtration. The thus obtained filtrate was extracted with ethyl acetate, washed with water and saturated brine and then dried over anhydrous sodium sulfate. The solvent was evaporated under a reduced pressure and the resulting residue was washed with diethyl ether to give 0.74 g of 2,4-dimethoxy-5-mercaptobenzoic acid.

1. temperatureUnder ice-cooling
2. temperaturethe mixture was then heated
3. temperatureunder reflux
4. customAfter completion of the reaction
5. customwas removed by celite filtration
6. extractionThe thus obtained filtrate was extracted with ethyl acetate
7. washwashed with water and saturated brine
8. dry with materialdried over anhydrous sodium sulfate
9. customThe solvent was evaporated under a reduced pressure
10. washthe resulting residue was washed with diethyl ether