反应详情

To a solution of N—((R)-piperidin-3-yl)-1-(4-(trifluoromethyl)phenyl)-3,4-dihydro-isoquinoline-2(1H)-carboxamide (30 mg, 74 μmol, example 24) in DCE (0.5 mL) was added formaldehyde (28 μL, 372 mol). The resulting mixture was stirred at RT for 1 h and then sodium triacetoxyborohydride (16 mg, 74 μmol) was added. The mixture was then stirred at RT for 4 h. Then, saturated NaHCO3 (0.4 mL) was added and the mixture was extracted with EtOAc (2×3 mL). The combined organic extracts were dried over MgSO4 and concentrated. The residue was purified by silica gel flash column chromatography (0%-10% MeOH (2M NH3)/EtOAc) to give the title compound as an off-white solid. MS (ESI, positive ion) m/z: 418 (M+H).

1. stirringThe mixture was then stirred at RT for 4 h
2. extractionthe mixture was extracted with EtOAc (2×3 mL)
3. dry with materialThe combined organic extracts were dried over MgSO4
4. concentrationconcentrated
5. customThe residue was purified by silica gel flash column chromatography (0%-10% MeOH (2M NH3)/EtOAc)