反应详情

To a solution of the compound from Example 8, step 2 (100 mg 0.3 mmol) in CH2Cl2 was added acetic anhydride (0.1 mL) and triethylamine (0.4 mL) sequentially at rt. The reaction mixture was stirred at it for 1 h and poured onto water (100 mL). The precipitate was collected by filtration and washed with water to give the title compound (58 mg, 64%) as an off-white solid: MS (ESI) m/z 297 (M+H); 1H NMR (400 MHz, CDCl3) δ 2.15 (s, 3H), 3.12 (m, 4H), 3.63 (t, J=5.2 Hz, 2H), 3.78 (t, J=5.2 Hz, 2H), 6.91-6.99 (m, 6H), 7.05 (m, 1H), 7.28-7.32 (m, 2H).

1. additionpoured onto water (100 mL)
2. filtrationThe precipitate was collected by filtration
3. washwashed with water