反应详情

To a solution of (6-amino-pyridin-3-yl)-(2-methoxy-phenyl)-methanone (14 g, 61.4 mol) in CH3OH (150 mL) was added NaBH4 (3.48 g, 92.1 mmol) portion-wise at 0° C. After the addition was completed, the reaction was warmed to room temperature and stirred at room temperature for 1 hr. The solvent was removed in vacuo and water (100 mL) was added to the residue. The mixture was extracted with dichloromethane (100 mL×3). The combined organic layers were washed with saturated solution of NaHCO3 and brine, dried over Na2SO4, filtered and concentrated in vacuo to give a crude product that was used directly in the next step with no further purification.

1. additionAfter the addition
2. customThe solvent was removed in vacuo and water (100 mL)
3. additionwas added to the residue
4. extractionThe mixture was extracted with dichloromethane (100 mL×3)
5. washThe combined organic layers were washed with saturated solution of NaHCO3 and brine
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo