反应详情

To a solution of tert-butyl 3-((3,5-dichloro-N-(4-(4-fluorophenoxy)benzyl)-2-hydroxyphenylsulfonamido)methyl)benzylcarbamate (0.98 g, 1.48 mmol) in CH2Cl2 (15 mL) was added TFA (2.28 mL, 29.6 mmol). The reaction mixture was stirred at rt for 3 h. The mixture was concentrated and the residue was partitioned between ethyl acetate and saturated NaHCO3 solution. The organic layer (clear solution) was washed with brine, dried over MgSO4 and concentrated to give white solid (0.65 g, 70%). 1H NMR (DMSO-d6): δ 8.50 (bs, 1H), 7.52 (s, 1H), 7.34 (d, J=2.8 Hz, 1H), 7.2.9 (d, J=2.8 Hz, 1H), 7.26-7.21 (m, 4H), 7.12-7.08 (m, 3H), 6.97-6.94 (m, 2H), 6.80 (d, J=6.8 Hz, 2H), 4.41 (s, 2H), 4.32 (s, 2H), 3.94 (s, 2H); MS (ESI): (M+H)+=561.1.

1. concentrationThe mixture was concentrated
2. customthe residue was partitioned between ethyl acetate and saturated NaHCO3 solution
3. washThe organic layer (clear solution) was washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated