反应详情

To 6-(1-formylisoquinolin-4-yloxy)nicotinamide (Preparation 20) (130 mg, 0.44 mmol) in dichloroethane (8 mL) was added 3-methylbutylamine (154 μL, 1.33 mmol), NaBH(OAc)3 (282 mg, 1.33 mmol) and acetic acid (76 μL, 1.33 mmol). The mixture was stirred for 16 h. NaHCO3 (50 mL) was added and the mixture extracted with EtOAc (3×40 mL). The organic phase was washed with water (30 mL), brine (30 mL) and dried (MgSO4). Solvent was removed in vacuo and the residue purified by column chromatography (0.5 NH3: 5 MeOH: 95 DCM) to give the title compound: RT=2.48 min; m/z (ES+)=365.2 [M+H]+.

1. extractionthe mixture extracted with EtOAc (3×40 mL)
2. washThe organic phase was washed with water (30 mL), brine (30 mL)
3. dry with materialdried (MgSO4)
4. customSolvent was removed in vacuo
5. customthe residue purified by column chromatography (0.5 NH3: 5 MeOH: 95 DCM)