反应详情

To a solution of 4-methyl-3-nitrobenzenesulfonyl chloride (5.40 g, 22.9 mmol) in chloroform (50 ml) was added tert-butylamine (6.00 ml, 57.1 mmol) under ice-cooling, and the mixture was stirred at room temperature for 2.5 hr. To the reaction mixture was added 1N hydrochloric acid, and the mixture was extracted with chloroform. The organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine, and dried over anhydrous sodium sulfate. After filtration, the solvent was evaporated under reduced pressure, and hexane was added to the residue. The precipitated solid was collected by filtration and dried in vacuo to give N-tert-butyl-4-methyl-3-nitrobenzenesulfonamide (5.89 g, yield 94.6%).

1. temperaturecooling
2. extractionthe mixture was extracted with chloroform
3. washThe organic layer was successively washed with water, saturated aqueous sodium hydrogen carbonate solution and saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. filtrationAfter filtration
6. customthe solvent was evaporated under reduced pressure, and hexane
7. additionwas added to the residue
8. filtrationThe precipitated solid was collected by filtration
9. customdried in vacuo