反应详情

NaH (35 mg, 0.91 mmol) was added to II (344 mg, 0.91 mmol) in DMF (5 mL) at rt. After 10 min, KI (227 mg, 1.37 mmol) and ethyl 7-bromoheptanoate (0.267 mL, 1.37 mmol) were added. The reaction mixture was stirred at 90° C. for 19 h after which 0.1 M Na2S2O3 (50 mL) and EtOAc (50 mL) were added; the phases were then separated and the aqueous phase extracted with EtOAc (2×25 mL). The organic phases were combined then dried over MgSO4, filtered, and subsequently evaporated under reduced pressure. The resulting residue was purified by silica gel column chromatography, eluting with hexane/EtOAc (90:10 to 85:15), to furnish III as a colourless oil (189 mg, 55%).

1. additionwere added
2. customthe phases were then separated
3. extractionthe aqueous phase extracted with EtOAc (2×25 mL)
4. dry with materialThe organic phases were combined then dried over MgSO4
5. filtrationfiltered
6. customsubsequently evaporated under reduced pressure
7. customThe resulting residue was purified by silica gel column chromatography
8. washeluting with hexane/EtOAc (90:10 to 85:15)