反应详情

A solution of ethyl 2,2-difluoro-3-iodo-3-(4-methoxyphenyl)-propionate (5.24 g, 14.2 mmol) in toluene (125 ml) was treated with tributyltin hydride (28.9 g, 0.10 mol) and a few crystals of 2,2′-azobisisobutyronitrile. The resulting solution was then irradiated for 15 minutes at 25° C. with a sun lamp. The solvent was then evaporated in vacuo and the residue was partitioned between acetonitrile and pentane. The acetonitrile fraction was concentrated and chromatographed on silica gel (elution hexane-ethyl acetate, 85:15) to give 2.65 g (76%) of the title material as an oil: bp 90-95° C./0.1 torr (air bath temperature).

1. customThe resulting solution was then irradiated for 15 minutes at 25° C. with a sun lamp
2. customThe solvent was then evaporated in vacuo
3. customthe residue was partitioned between acetonitrile and pentane
4. concentrationThe acetonitrile fraction was concentrated
5. customchromatographed on silica gel (elution hexane-ethyl acetate, 85:15)