反应详情

The product of Example 38I (1.0 g, 6.92 mmol) in CH2Cl2 (5 mL) was treated with trifluoroacetic acid (5 mL) at room temperature for 1 hour. The mixture was concentrated and the residue was diluted with CHCl3 (50 mL). The brown chloroform solution was washed with saturated aqueous NaHCO3 (2×20 mL, pH=8-9) and brine (5 mL), dried (MgSO4), filtered, and the filtrate concentrated to provide the title compound as a brown oil (0.64 g, 97% yield) which was used in the next step without purification. 1H NMR (MeOH-d4, 300 MHz) δ 3.30-3.16 (m, 3H), 3.36 (m, 1H), 3.80 (m, 3H), 4.45 (dd, J=6.4 Hz, 4.8 Hz, 1H), 5.16 (s, 2H), 7.36 (m, 5H); MS (DCI/NH3) m/z 250 (M+NH4)+, 233 (M+H)+.

1. concentrationThe mixture was concentrated
2. additionthe residue was diluted with CHCl3 (50 mL)
3. washThe brown chloroform solution was washed with saturated aqueous NaHCO3 (2×20 mL, pH=8-9) and brine (5 mL)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationthe filtrate concentrated