反应详情

温度

100 °C

A mixture of 2-(4-chloro-phenyl)-2-(4-iodo-phenyl)-oxirane* (571 mg, 1.60 mmol) and potassium phthalimide (340 mg, 1.84 mmol) in THF (5 mL) and DMSO (2 mL) was heated at 100° C. for 20 hours. The mixture was concentrated in vacuo, diluted with ethyl acetate and washed with water and brine (×2), dried (MgSO4), filtered and concentrated to give a crude product which was purified by column chromatography (SiO2), eluting with a gradient of ethyl acetate/petrol (2.5% to 100%) then 10% methanol/dichloromethane to give the title compound (273 mg, 34%); LCMS (PS-A2) Rt 3.22 min [M+H]+504. *This starting material can be made by the method described in Example 79A

1. concentrationThe mixture was concentrated in vacuo
2. additiondiluted with ethyl acetate
3. washwashed with water and brine (×2)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. customto give a crude product which
8. customwas purified by column chromatography (SiO2)
9. washeluting with a gradient of ethyl acetate/petrol (2.5% to 100%)