反应详情

The product of Example J (1.6 g, 0.006 mole) was dissolved in 30 mls of dry DMF at room temperature under a nitrogen atmosphere and potassium t-butoxide (1.4 g) was added. After stirring for 5 minutes, 1 g of allyl iodide was added and the reaction was warmed to +50° C. for 1 hour. Another half equivalent of allyl iodide was added and the stirring was continued for 2 hours at +50° C. After cooling to room temperature the mixture was poured into 50 mls of 0.5N KHSO4 and extracted with ethyl acetate. After drying the organic layer over Na2SO4, the solvent was removed and the residue was chromatographed on silica gel using 10% ethyl acetate/hexane to give 1 g of the title compound (54% yield).

1. temperaturethe reaction was warmed to +50° C. for 1 hour
2. waitthe stirring was continued for 2 hours at +50° C
3. extractionextracted with ethyl acetate
4. dry with materialAfter drying the organic layer over Na2SO4
5. customthe solvent was removed
6. customthe residue was chromatographed on silica gel using 10% ethyl acetate/hexane