反应详情

To a solution of 1-benzylindolin-5-yl 4-isopropylphenylcarbamate (300 mg, 0.776 mmol) in a 2:1 solution (3.0 mL) of isopropylalcohol and 6 M HCl was added palladium 10% on carbon (30 mg) under nitrogen. After the vessel was purged with hydrogen, the reaction mixture was stirred under 1 atm of hydrogen at room temperature overnight. After the vessel was purged with nitrogen, the reaction mixture was filtered to remove palladium 10% on carbon. The filtrate was concentrated in vacuo. After the residue was diluted with ethyl acetate, the solution was washed with saturated NaHCO3 aqueous solution, brine, and dried over MgSO4. After filtration, the filtrate was concentrated in vacuo, and the residue was purified by silica gel column chromatography (hexane/ethyl acetate=85/15 to 40/60) to obtain the title compound as a white solid (220 mg, 96%).

1. customAfter the vessel was purged with hydrogen
2. customAfter the vessel was purged with nitrogen
3. filtrationthe reaction mixture was filtered
4. customto remove palladium 10% on carbon
5. concentrationThe filtrate was concentrated in vacuo
6. additionAfter the residue was diluted with ethyl acetate
7. washthe solution was washed with saturated NaHCO3 aqueous solution, brine
8. dry with materialdried over MgSO4
9. filtrationAfter filtration
10. concentrationthe filtrate was concentrated in vacuo
11. customthe residue was purified by silica gel column chromatography (hexane/ethyl acetate=85/15 to 40/60)