反应详情

A mixture of N-[(1S,2S,4R)-1-Benzyl-4-(3,3-bimethylbutylcarbamoyl)-2-hydroxypentyl]-3-hydroxy-5-(2-oxopyrrolidin-1-yl)-benzamide (E2) (0.061 g, 0.117 mmol), caesium carbonate (0.050 g, 0.152 mmol) and allyl bromide (0.016 ml, 0.176 mmol) in DMF (1 ml) was stirred vigorously at room temperature for 2 hrs. More allyl bromide (0.008 ml) was added and stirring was continued for a further 1 hr. The mixture was diluted with ethyl acetate and 2N HCl and the product was extracted into ethyl acetate. The combined extracts were washed with brine, dried over sodium sulfate and evaporated. Purification by column chromatography on silica gel (elution with 2–5% methanol in dichloromethane) gave the product, 0.047 g.

1. stirringstirring
2. waitwas continued for a further 1 hr
3. extractionthe product was extracted into ethyl acetate
4. washThe combined extracts were washed with brine
5. dry with materialdried over sodium sulfate
6. customevaporated
7. customPurification by column chromatography on silica gel (elution with 2–5% methanol in dichloromethane)
8. customgave the product, 0.047 g