反应详情

To a solution of Intermediate 81b (657 mg, 2.60 mmol), Ph3P (1.37 g, 5.21 mmol) and Et3N (1.45 mL, 10.4 mmol) in THF (20 mL) at 0° C. was added hexachloroethane (1.23 g, 5.21 mmol) and the resulting yellow suspension was stirred at RT for 2 h, and at reflux for 19 h. The cooled solution was filtered and concentrated in vacuo. The brown oil was redissolved in MeOH (3 mL) and applied to an SCX-2 cartridge (20 g), washing with MeOH (100 mL). The product was eluted with 2M NH3 in MeOH (75 mL); concentration in vacuo gave a brown oil. FCC, using 1-5% [2M NH3 in MeOH] in DCM, gave the title compound as a brown oil (542 mg, 89%). LCMS (Method 3): Rt 3.00 min, m/z 235 [MH+].

1. temperatureat reflux for 19 h
2. filtrationThe cooled solution was filtered
3. concentrationconcentrated in vacuo
4. dissolutionThe brown oil was redissolved in MeOH (3 mL)
5. washwashing with MeOH (100 mL)
6. washThe product was eluted with 2M NH3 in MeOH (75 mL)
7. concentrationconcentration in vacuo
8. customgave a brown oil