反应详情

温度

0 °C

To a solution of Intermediate 47a (668 mg, 2.64 mmol), Et3N (1.5 mL, 11 mmol) and Ph3P (1.4 g, 5.3 mmol) in THF (20 mL) at 0° C. was added hexachloroethane (1.25 g, 5.29 mmol). The mixture was stirred at 0° C. for 10 min, then at RT for 1 h. The mixture was partitioned between EtOAc/water and the aqueous extracted with EtOAc. The combined organics were dried (Na2SO4), filtered and concentrated in vacuo. Purification by FCC, using 0-10% MeOH in EtOAc, gave the title compound as a pale brown solid (300 mg, 49%). LCMS (Method 4): Rt 0.39, m/z 235 [MH+].

1. waitat RT for 1 h
2. customThe mixture was partitioned between EtOAc/water
3. extractionthe aqueous extracted with EtOAc
4. dry with materialThe combined organics were dried (Na2SO4)
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customPurification by FCC