反应详情

温度

80 °C

To a solution of [7-Benzyloxy-2-methyl-4-(5-methyl-chroman-6-yl)-1-oxo-1,2-dihydro-isoquinolin-3-yl]-trimethylsilanyloxy-acetonitrile (2.5 g, 4.64 mmol) in H2SO4/CH3OH (30 mL, V/V=1:3). The resulting mixture was heated to 80° C. under N2 for 12 h. The reaction mixture was poured into ice water and extracted with DCM (50 mL*3), dried over sodium sulfate and concentrated to dryness. The mixture was purified by chromatography column on silica gel to afford the title product (0.6 g, 32%). LCMS (10-80 AB—2MIN.M): Rt=0.993, purity=75%, M+1=410.

1. extractionextracted with DCM (50 mL*3)
2. dry with materialdried over sodium sulfate
3. concentrationconcentrated to dryness
4. customThe mixture was purified by chromatography column on silica gel