反应详情

To compound H (335 mg, 0.99 mmol) in ethanol (5 mL) cooled to 0° C. was added sodium borohydride (18.7 mg, 0.49 mmol). After ten minutes, the reaction was diluted with EtOAc and washed well with water. The organic layer was dried (MgSO4), filtered and concentrated in vacuo. Purification by flash chromatography on silica gel afforded 192 mg (57%) of the title compound. 1H NMR (400 MHz, DMSO-d6) δ 8.44 (s, 1H), 8.25 (s, 1H), 7.76-7.72 (m, 2H), 7.61 (d, J=6 Hz, 1H), 7.54 (t, J=8.64, 8.68 Hz, 2H), 6.94 (d, J=8.68, 1H), 5.42 (t, J=5.68, 5.64 Hz, 1H), 4.62 (d, J=5.48 Hz, 2H), 4.23 (q, J=7.08 Hz, 2H), 1.27 (t, J=7.12, 7.04 Hz, 3H); ES-MS [M+1]+: 342.3.

1. waitAfter ten minutes
2. washwashed well with water
3. dry with materialThe organic layer was dried (MgSO4)
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customPurification by flash chromatography on silica gel