反应详情

To a solution of Intermediate 83a (375 mg, 1.10 mmol), Ph3P (578 mg, 2.20 mmol) and Et3N (614 μL, 4.41 mmol) in THF (11.0 mL) at 0° C. was added hexachloroethane (523 mg, 2.20 mmol). The reaction was stirred at RT overnight then partitioned between EtOAc and water. The aqueous layer was then extracted with EtOAc (3×). The combined organic layers were washed with brine, dried (MgSO4), filtered and evaporated in vacuo. The residue was taken up in MeOH and loaded onto an SCX-2 cartridge, which was washed with MeOH and eluted with 2M NH3 in MeOH; concentration in vacuo gave the title compound (297 mg, 84%). LCMS (Method 1): Rt 2.73, m/z 323.2 [MH+].

1. customthen partitioned between EtOAc and water
2. extractionThe aqueous layer was then extracted with EtOAc (3×)
3. washThe combined organic layers were washed with brine
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated in vacuo
7. washwas washed with MeOH
8. washeluted with 2M NH3 in MeOH
9. concentrationconcentration in vacuo