反应详情

温度

60 °C

To a suspension of NaH (60% in mineral oil, 51.0 mg, 1.27 mmol) in DMF (1.50 mL) was added Intermediate A (51.0 mg, 0.32 mmol) and the reaction stirred for 20 min. Intermediate 83c (75.0 mg, 0.32 mmol) was added in DMF (1.50 mL) and the reaction heated to 60° C. for 1 h. The reaction was cooled and quenched by dropwise addition of methanol, before being diluted with methanol and loaded onto an SCX-2 cartridge, which was 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 (31 mg, 26%). LCMS (Method 4): Rt 0.32, in/z 380.0 [MH+].

1. temperatureThe reaction was cooled
2. customquenched by dropwise addition of methanol
3. additionbefore being diluted with methanol
4. washwas washed with MeOH
5. washThe product was eluted with 2M NH3 in MeOH
6. concentrationconcentration in vacuo
7. customgave a residue