反应详情

A solution of 3.52 g (18.3 mmol) of 13 in 50 mL toluene was treated with methyl(triphenylphosphoranylidene)acetate (7.48 g, 21.9 mmol). After 4 h, saturated NaHCO3 solution (50 mL) was added and the mixture extracted with ethyl acetate (2×75 mL). The combined ethyl acetate solution was washed with brine (50 mL), dried (Na2SO4), filtered and evaporated. Purification by flash chromatography on silica gel (5% ethyl acetate/hexane) provided 3.60 g (14.6 mmol, 80%) of the enoate (14).

1. extractionthe mixture extracted with ethyl acetate (2×75 mL)
2. washThe combined ethyl acetate solution was washed with brine (50 mL)
3. dry with materialdried (Na2SO4)
4. filtrationfiltered
5. customevaporated
6. customPurification by flash chromatography on silica gel (5% ethyl acetate/hexane)