反应详情

A mixture of 9.37 g of 2,3 dichloro-4-methoxybenzenesulfonyl chloride, 72 g of crushed ice, 24 g of conc. sulfuric acid and 12 g of zinc dust is stirred under reflux for 16 hours. The mixture is diluted with dichloromethane, cooled and stirred at room temperature for 2 hours. Filtration removes the unreacted zinc and the organic extracts are washed with water, sodium bicarbonate solution and dried over anhydrous magnesium sulfate. Removal of solvent in vacuo leaves a white solid which is recrystallized from ether-pentane to give 5.5 g of 2,3-dichloro-4-methoxy-thiophenol as colorless needles, mp 81.5°-83°.

1. temperatureunder reflux for 16 hours
2. temperaturecooled
3. stirringstirred at room temperature for 2 hours
4. filtrationFiltration
5. customremoves the unreacted zinc
6. washthe organic extracts are washed with water, sodium bicarbonate solution
7. dry with materialdried over anhydrous magnesium sulfate
8. customRemoval of solvent in vacuo
9. customleaves a white solid which
10. customis recrystallized from ether-pentane