反应详情

To a stirred solution of 1,2,3,4-tetrahydro-9H-pyrido[3,4-b]indole (20.0 g, 116.2 mmole) in dry DMF (150 mL) at RT was added N-(benzyloxycarbonyloxy)succinimide (31.84 g, 127.76 mmole) and triethylamine (13.0 g. 127.76 mmole). After 12 h, the reaction contents were poured into H2O (150 mL) and extracted with EtOAc (2×200 mL). The combined organic phases were washed sequentially with H2O and brine, then were dried over Na2SO4. Concentration under reduced pressure gave a yellow oil. Purification on silica (hexanes/EtOAc, 4:1) afforded the title compound (34.48 g. 97%) as a white solid: MS (ES) m/e 307 (M+H)+.

1. customthe reaction contents
2. extractionextracted with EtOAc (2×200 mL)
3. washThe combined organic phases were washed sequentially with H2O and brine
4. dry with materialwere dried over Na2SO4
5. concentrationConcentration under reduced pressure
6. customgave a yellow oil
7. customPurification on silica (hexanes/EtOAc, 4:1)