反应详情

温度

90 °C

To a solution of 4-chloro-2-methoxybenzamide (0.82 g, 4.42 mmol) in toluene (20 ml) was added chlorocarbonylsulfenyl chloride (0.73 ml, 8.84 mmol) under nitrogen atmosphere and the resulting reaction mixture was refluxed at 90° C. for 2 h. After the completion of the reaction (TLC monitoring) water was added followed by extraction with ether (3×50 ml). The combined organics was then sequentially washed with water, 10% NaHCO3 (aqueous solution) and finally again with water. The organic layer was then dried over anhydrous Na2SO4, filtered and concentrated to get desired product (1.03 g, 96% crude yield) that was carried forward as such without further purification. MS: 244.16 (M+H)+.

1. customthe resulting reaction mixture
2. additionwas added
3. extractionfollowed by extraction with ether (3×50 ml)
4. washThe combined organics was then sequentially washed with water, 10% NaHCO3 (aqueous solution) and finally again with water
5. dry with materialThe organic layer was then dried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated