反应详情

温度

0 °C

A solution of Example 21 step a (0.41 g, 2.08 mmol), triphenylphosphine (763 mg, 2.91 mmol) and triethylamine (0.87 mL, 6.24 mmol) in THF (5 mL) at 0° C. was treated with 1,2-hexachloroethane (690 mg, 2.91 mmol). The reaction mixture was stirred at 0° C. for 40 min then at RT for 20 min, quenched with water, extracted twice with EtOAc, dried (Na2SO4), evaporated and purified twice by FCC (cyclohexane/EtOAc 1/0 to 1/1) to afford the title compound (274 mg, contaminated with 20% PPh3O, 58%) as a white solid. LCMS (Method 5): Rt 2.58 min, m/z 180 [MH+].

1. waitat RT for 20 min
2. customquenched with water
3. extractionextracted twice with EtOAc
4. dry with materialdried (Na2SO4)
5. customevaporated
6. custompurified twice by FCC (cyclohexane/EtOAc 1/0 to 1/1)