反应详情

To a solution of 2-methylcarbamoyl-isonicotinic acid ethyl ester (7.77 g, 37.3 mmol) in absolute ethanol (125 mL) was added sodium borohydride (2.82 g, 74.6 mmol, 2.0 eq), and the reaction mixture was stirred at RT under argon for 18 h. The solvent was evaporated under reduced pressure, and the residue was partitioned between EtOAc and water. The aqueous layer was extracted with EtOAc (2×100 mL), and the combined organic layers were dried over Na2SO4, filtered, and concentrated at reduced pressure to give 5.36 g (86.5%) of 4-(hydroxymethyl)-N-methylpyridine-2-carboxamide as a colorless solid: MS LC-MS [M+H]+=153.

1. customThe solvent was evaporated under reduced pressure
2. customthe residue was partitioned between EtOAc and water
3. extractionThe aqueous layer was extracted with EtOAc (2×100 mL)
4. dry with materialthe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated at reduced pressure