反应详情

温度

0 °C

A solution of 7 (170 mg, 0.28 mmol) in 4 mL toluene was added, by cannula, to a −40° C. mixture of hydrido(triphenylphosphine)copper(I) hexamer (300 mg, 0.15 mmol) in 4 mL toluene, rinsing with 0.5 mL toluene. The temperature was allowed to warm to 0° C. over 1 h and then was allowed to warm to room temperature. After a further 1 h, the reaction was quenched by addition of 15 mL saturated NH4Cl solution. The mixture was extracted with ethyl acetate (3×15 mL) and the combined ethyl acetate solution was dried (Na2SO4), filtered and evaporated. Purification by flash chromatography (8% ethyl acetate/hexanes→10%) gave the title ketone (150 mg, 0.25 mmol, 89%).

1. washrinsing with 0.5 mL toluene
2. temperatureto warm to room temperature
3. customthe reaction was quenched by addition of 15 mL saturated NH4Cl solution
4. extractionThe mixture was extracted with ethyl acetate (3×15 mL)
5. dry with materialthe combined ethyl acetate solution was dried (Na2SO4)
6. filtrationfiltered
7. customevaporated
8. customPurification by flash chromatography (8% ethyl acetate/hexanes→10%)