反应详情

Compound 75a (74.5 mg, 0.223 mmol) was suspended in MeOH (10 mL) and then NaBH4 (26.3 mg, 0.695 mmol) was added. The reaction was stirred at rt for 18 h and then diluted with water (10 mL) and filtered. The solid was collected by filtration and the filter cake was washed with water (2×10 mL). The solid was dissolved in a mixture of DCM (100 mL) and MeOH (50 mL), dried over Na2SO4, and filtered. The solvent was removed under reduced pressure to afford compound 75b. 1H-NMR (400 MHz, CD3OD+CDCl3) δ (ppm): 8.96 (d, J=2.2 Hz, 1H), 8.20 (dd, J=8.1, 2.2 Hz, 1H), 7.95 (d, J=8.1 Hz, 1H), 7.70 (s, 1H), 7.43 (s, 1H), 4.79 (s, 2H), 4.29-4.36 (m, 4H), 3.85-3.94 (m, 4H). LCMS calcd for C17H16N6O2: 337.1 (M+H). found: 337.1.

1. filtrationfiltered
2. filtrationThe solid was collected by filtration
3. washthe filter cake was washed with water (2×10 mL)
4. dissolutionThe solid was dissolved in a mixture of DCM (100 mL) and MeOH (50 mL)
5. dry with materialdried over Na2SO4
6. filtrationfiltered
7. customThe solvent was removed under reduced pressure