反应详情

温度

60 °C

To a suspension of sodium hydride (60% in mineral oil, 133 mg, 3.34 mmol) in DMF (5 mL) was added Intermediate A (136 mg, 0.83 mmol) and the reaction mixture was stirred for 20 min. A solution of Intermediate 99c (207 mg, 0.83 mmol) in DMF (3 mL) was added and the reaction mixture was heated at 60° C. for 90 min. After cooling, the reaction mixture was quenched by careful addition of MeOH and then loaded onto an SCX cartridge. The cartridge was washed with MeOH and the product eluted with 2M NH3 in MeOH. The product containing fractions were concentrated in vacuo and the resultant residue was purified by FCC on silica, using a gradient of 0-10% (2M NH3 in MeOH) in DCM, to give the title compound (211 mg, 65%). LCMS (Method 4): Rt 1.49 min, m/z 392 [MH+].

1. temperatureAfter cooling
2. customthe reaction mixture was quenched by careful addition of MeOH
3. washThe cartridge was washed with MeOH
4. washthe product eluted with 2M NH3 in MeOH
5. additionThe product containing fractions
6. concentrationwere concentrated in vacuo
7. customthe resultant residue was purified by FCC on silica