反应详情

To a solution of the product of Example 111-5 in dichloromethane (1.5 L) was added triflouroacetic acid (810 mL). The mixture was stirred at room temperature for 3 hours and concentrated. The residue was chased with heptanes (4×500 mL). The product was partitioned between dichloromethane (1.5 L) and 5% KH2PO4 (1.1 L). The organic layer was washed with 5% KH2PO4 (900 mL) and brine (900 mL), and concentrated. A solution of the residue in dichloromethane (500 mL) was dried over MgSO4, filtered and concentrated. The residue was recrystallized twice from isopropyl alcohol/water to afford the title compound. 1H NMR (DMSO-d6): δ 7.2-7.4(m, 5H), 4.28(d, 2H), 4.21(s, 1H), 3.47-3.64(m, 2H), 3.08-3.2(m, 2H), 1.0(s, 9H).

1. concentrationconcentrated
2. customThe product was partitioned between dichloromethane (1.5 L) and 5% KH2PO4 (1.1 L)
3. washThe organic layer was washed with 5% KH2PO4 (900 mL) and brine (900 mL)
4. concentrationconcentrated
5. dry with materialA solution of the residue in dichloromethane (500 mL) was dried over MgSO4
6. filtrationfiltered
7. concentrationconcentrated
8. customThe residue was recrystallized twice from isopropyl alcohol/water