反应详情

4-Amino-7-[1-(tert-butoxycarbonyl)-5-(piperidinomethyl)indol-2-yl]isoindolinone (0.0820 g, 0.178 mmol) was dissolved in dichloromethane (4.0 mL), and the solution was added with pyridine (0.0430 mL, 0.534 mmol) and methanesulfonyl chloride (0.0210 mL, 0.267 mmol), followed by stirring for 1.5 hours under ice-cooling. The reaction mixture was added with water and extracted with ethyl acetate. The organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by flash column chromatography (chloroform/methanol=4/1) to obtain 4-methanesulfonylamino-7-[1-(tert-butoxycarbonyl)-5-(piperidinomethyl)indol-2-yl]isoindolinone (0.0423 g, yield 44%).

1. temperaturecooling
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed with saturated brine
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by flash column chromatography (chloroform/methanol=4/1)