反应详情

To a solution of 29-3 (100 mg, 0.24 mmol) in THF (10 mL) was added lithium aluminum hydride (19 mg, 0.48 mmol). The mixture was stirred at room temperature overnight. Na2SO4.10H2O was added and the reaction mixture was filtered and the filtrate was evaporated to give the crude product which was purified by preparative HPLC (basic condition, water/CH3CN, 43-53% CH3CN in 7.5 min, RT=7.3 min) to afford 29-4 (22 mg, 23%) as a yellow solid. 1H-NMR (400 MHz, CDCl3): δ (ppm) 7.52-7.50 (br.s, 2H), 7.20-7.16 (m, 2H), 6.76 (s, 1H), 6.66 (d, J=12.8 Hz, 1H), 3.96 (q, J=7.2 Hz, 2H), 3.81 (s, 3H), 3.14 (t, J=7.2 Hz, 2H), 3.06-2.98 (m, 4H), 2.69 (t, J=7.6 Hz, 2H), 2.38 (s, 6H) 1.30 (t, J=7.2 Hz, 3H). LRMS: calc 408.5 and found: 409.2 [M+1].

1. filtrationthe reaction mixture was filtered
2. customthe filtrate was evaporated
3. customto give the crude product which
4. customwas purified by preparative HPLC (basic condition, water/CH3CN, 43-53% CH3CN in 7.5 min, RT=7.3 min)