反应详情

To a solution of tert-butyl 4-{[4-({[(2′-oxospiro[cyclopentane-1,3′-indol]-1′(2′H)-yl)carbonyl]amino}methyl)piperidin-1-yl]methyl}tetrahydro-2H-pyran-4-carboxylate (2.3 g, 4.38 mmol, step 6 of Example 1) in CH2Cl2 (14 mL), trifluoroacetic acid (18 mL) was added at room temperature, and the mixture was stirred overnight at room temperature. The mixture was concentrated to give yellow oil, CH2Cl2 (200 mL) was added and washed with sat. NaHCO3 aq. (80 mL), dried over MgSO4, filtered and concentrated gave a syrup, which was chromatographed on a column of silica gel eluting with CH2Cl2/methanol (15:1) to give 2.1 g (quant.) of the title compound as white solid. Recrystallization from ethyl acetate/n-heptane gave white powder.

1. concentrationThe mixture was concentrated
2. customto give yellow oil, CH2Cl2 (200 mL)
3. additionwas added
4. washwashed with sat. NaHCO3 aq. (80 mL)
5. dry with materialdried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customgave a syrup, which
9. customwas chromatographed on a column of silica gel eluting with CH2Cl2/methanol (15:1)