反应详情

To a solution of compound 41 (0.74 mmol) in dichloroethane (700 mL), degassed for 45 min by bubbling nitrogen, was Zhan 1B (4%, 22 mg) at 80° C. under continuous degassing with nitrogen. After the reaction was refluxed for 1 hr, a second portion of Zhan 1B (22 mg) was added. After heating for 1.5 hr, the reaction mixture was cooled down to room temperature, poured onto a silica pad, and eluted with DCM. The crude material was purified by chromatography on silica gel (DCM/MeOH) to yield compound 42 as a brown solid in 81% yield. MS (ESI, EI+): m/z=617 (MH+).

1. customby bubbling nitrogen
2. customat 80° C.
3. customunder continuous degassing with nitrogen
4. temperatureAfter the reaction was refluxed for 1 hr
5. additiona second portion of Zhan 1B (22 mg) was added
6. temperatureAfter heating for 1.5 hr
7. additionpoured onto a silica pad
8. washeluted with DCM
9. customThe crude material was purified by chromatography on silica gel (DCM/MeOH)