反应详情

温度

60 °C

Intermediate B (74.0 mg, 454 μmol) was added to a mixture of NaH (60% in mineral oil, 27.2 mg, 681 μmol) in DMF (2.5 mL) at RT and stirred for 15 min. Intermediate 3b (100 mg, 454 μmol) was then added and the resulting mixture heated to 60° C. for 1 h. After cooling, the reaction was quenched with sat. aq. NH4Cl solution. The mixture was diluted with water and extracted with EtOAc. The combined organic extracts were concentrated in vacuo. The resulting residue was purified by FCC, using 0 to 10% [2M NH3 in MeOH] in DCM, to afford the title compound as an orange residue (122 mg, 74%). LCMS (Method 3): Rt 2.13 min, m/z 364 [MH+].

1. temperatureAfter cooling
2. customthe reaction was quenched with sat. aq. NH4Cl solution
3. additionThe mixture was diluted with water
4. extractionextracted with EtOAc
5. concentrationThe combined organic extracts were concentrated in vacuo
6. customThe resulting residue was purified by FCC