反应详情

To the mixture of 4-aminonicotinic acid (691 mg, 5.0 mmol), methylamine hydrogen chloride (410 mg, 1.2 eq), EDC (1.15 g, 1.2 eq), HOBt (810 mg, 1.2 eq) in DMF (20 mL) was added DIEA (3.0 mL, 3.0 eq). The mixture was stirred at room temperature overnight. It was concentrated and dissolved in EtOAc. It was washed with saturated NaHCO3 solution. It was concentrated and purified by silica gel with chromatography (0%˜20% MeOH/DCM) to obtain the desired product 4-amino-N-methylnicotinamide.

1. concentrationIt was concentrated
2. dissolutiondissolved in EtOAc
3. washIt was washed with saturated NaHCO3 solution
4. concentrationIt was concentrated
5. custompurified by silica gel with chromatography (0%˜20% MeOH/DCM)