反应详情

温度

40 °C

To a stirred suspension of methyltriphenylphosphonium bromide (8.48 g, 23.7 mmol) in THF (75 ml) was added potassium tert-butoxide (2.66 g, 23.7 mmol) at room temperature. The mixture was stirred at 40° C. for 1 hour. After cooling to room temperature, a solution of 2-[4-tert-butylphenyl]-2-oxoethyl acetate (U.S. Pat. No. 3,526,634, 2.78 g, 11.9 mmol) in THF (25 ml) was added to the mixture. The mixture was heated at reflux for 3 hours. The mixture was concentrated, diluted with EtOAc and washed with water and brine. The organic layer was dried over sodium sulfate and concentrated in vacuo. The crude material was purified by silica gel column chromatography, eluting with hexane/EtOAc (9:1), to afford the title compound (2.13 g, 77%) as a yellow oil.

1. temperatureAfter cooling to room temperature
2. temperatureThe mixture was heated
3. temperatureat reflux for 3 hours
4. concentrationThe mixture was concentrated
5. additiondiluted with EtOAc
6. washwashed with water and brine
7. dry with materialThe organic layer was dried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customThe crude material was purified by silica gel column chromatography
10. washeluting with hexane/EtOAc (9:1)