反应详情

Compound 9 (5.0 g, 11.9 mmol) was suspended in anhydrous ethanol (60 mL) at room temperature and sodium borohydride (0.23 g, 6.1 mmol) was added with efficient stirring. Reaction was complete in 1 h, solvent was evaporated and the residue was dissolved in ethyl acetate. The organic layer was extracted with water (50 mL), brine (25 mL), dried on anhydrous magnesium sulfate, filtered and solvent was evaporated to yield the title compound 12 as white solid (5.1 g, 100%): mp 93-95° C.; 1H NMR (400 MHz, DMSO-d6) δ 7.72 (s, 1H), 7.35 (d, J=8.8 Hz, 2H), 7.19 (d, J=8.8 Hz, 2H), 7.02 (d, J=8.4 Hz, 2H), 7.00 (d, J=8.4 Hz, 2H), 6.41 (t, J=2.4 Hz, 1H), 6.29 (d, J=2.0 Hz, 2H), 5.18 (t, J=6.4 Hz, 1H), 4.49 (d, J=4.8 Hz, 2H), 3.73 (s, 3H), 3.57 (s, 6H); MS (EI) m/z 315[M]+. Anal. (C25H24O6) C, H.

1. customReaction
2. customsolvent was evaporated
3. dissolutionthe residue was dissolved in ethyl acetate
4. extractionThe organic layer was extracted with water (50 mL), brine (25 mL)
5. dry with materialdried on anhydrous magnesium sulfate
6. filtrationfiltered
7. customsolvent was evaporated