反应详情

温度

55 °C

To a solution of tert-butyl 3-((4-oxo-1-phenyl-1,3,8-triazaspiro[4.5]decan-3-yl)methyl)benzoate (1.2 g, 2.84 mmol) and potassium carbonate (0.59 g, 4.3 mmol) in N,N-dimethylformamide (20 mL), was added 1-(3-iodopropyl)-1,3-dihydro-2H-benzimidazol-2-one (0.86 g, 2.84 mmol). After stirring at 55° C. for 5 hours, the reaction mixture was diluted with ethyl acetate (100 mL), washed with water and brine. The organic phase was dried over MgSO4, filtered, concentrated and isolated by Biotage flash chromatography (2-10% methanol/dichloromethane) to obtain the title compound (1 g, 59%); 1H NMR (DMSO-d6): δ 1.51 (s, 9H), 1.60 (d, 2H, J=13.2 Hz), 1.82 (t, 2H, J=6.4 Hz), 2.35 (t, 2H, J=6.4 Hz), 2.53-2.60 (m, 4H), 2.65-2.71 (m, 4H), 3.85 (t, 2H, J=6.8 Hz), 4.56-4.60 (m, 2H), 6.76 (t, 1H, J=14.4 Hz), 6.85 (d, 2H, J=8 Hz), 6.95-6.97 (m, 3H), 7.17-7.24 (m, 3H), 7.48-7.54 (m, 2H), 7.78 (s, 1H), 7.82 (dt, 1H, J=7.2 and 1.6 Hz) 10.81 (s, 1H); MS for C35H41N5O4 m/z 596 (M+H)+.

1. washwashed with water and brine
2. dry with materialThe organic phase was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated
5. customisolated by Biotage flash chromatography (2-10% methanol/dichloromethane)