反应详情

To a solution of 5-Methoxy-2-nitro-phenylamine (5.0 g, 0.030 mol) and Triethylamine (10.0 mL, 0.0717 mol) in Methylene chloride (100 mL, 2 mol) at 0° C. was added dropwise Methanesulfonyl chloride (5.1 mL, 0.065 mol). The mixture was stirred for 18 hours. The mixture was poured into 1N Hydrochloric Acid (200 mL). The aqueous was extracted with dichloromethane (3×100 mL). The combined organic layers were dried over magnesium sulfate, filtered and evaporated. The oil was purified by silica gel chromatography using 20%→100% Ethyl Acetate:Hexane solvent gradient. N-(5-Methoxy-2-nitro-phenyl)-N-(methylsulfonyl) methanesulfonamide isolated as a yellow solid (7.75 g, 80%).

1. extractionThe aqueous was extracted with dichloromethane (3×100 mL)
2. dry with materialThe combined organic layers were dried over magnesium sulfate
3. filtrationfiltered
4. customevaporated
5. customThe oil was purified by silica gel chromatography