反应详情

温度

60 °C

To a solution of Intermediate 47b (150 mg, 0.64 mmol) and Intermediate A (126 mg, 0.64 mmol) in DMF (3 mL) was added NaH (60% in mineral oil, 90 mg, 2.24 mmol) portionwise. The mixture was stirred at 60° C. for 1.5 h then allowed to cool to RT. The mixture was carefully quenched by pouring into MeOH (10 mL), then applied to an SCX-2 cartridge and washed with MeOH. The product was eluted with 2M NH3 in MeOH; concentration in vacuo gave a residue. FCC, using 0-10% [2M NH3 in MeOH] in DCM, gave the title compound as a brown solid (180 mg, 75%). LCMS (Method 4): Rt 0.49, m/z 378 [MH+].

1. temperatureto cool to RT
2. customThe mixture was carefully quenched
3. additionby pouring into MeOH (10 mL)
4. washwashed with MeOH
5. washThe product was eluted with 2M NH3 in MeOH
6. concentrationconcentration in vacuo
7. customgave a residue