反应详情

A mixture of Intermediate A (44 mg, 0.267 mmol) and sodium hydride (60% in mineral oil, 29 mg, 0.729 mmol) in anhydrous DMF (1 mL) was stirred at RT for 20 min under argon atmosphere. To the reaction mixture was added a solution of Intermediate 105d (57 mg, 0.243 mmol) in anhydrous DMF (2 mL) and stirring at 60° C. was continued for 2.5 h. After cooling to RT, the reaction mixture was diluted with EtOAc and poured into ice-water. The aqueous phase was extracted with EtOAc (×3) and the combined organic layers were dried (MgSO4) and concentrated in vacuo. The resultant residue was purified by SCX cartridge by washing the cartridge with 10% MeOH in DCM and eluting the product with 10% (2M NH3 in MeOH) in DCM and then by FCC on silica, using 10% MeOH in DCM followed by 10% [2M NH3 in MeOH] in DCM, to give the title compound (53 mg, 58%). LCMS (Method 1): Rt 0.38, 1.54 min, m/z 378 [MH+].

1. stirringstirring at 60° C.
2. waitwas continued for 2.5 h
3. temperatureAfter cooling to RT
4. extractionThe aqueous phase was extracted with EtOAc (×3)
5. dry with materialthe combined organic layers were dried (MgSO4)
6. concentrationconcentrated in vacuo
7. customThe resultant residue was purified by SCX cartridge
8. washby washing the cartridge with 10% MeOH in DCM
9. washeluting the product with 10% (2M NH3 in MeOH) in DCM