反应详情

温度

-65 °C

A -30° C. solution of bromotrifluoroethylene (7.15 g, 0.044 mol) in ether is treated with p-(chlorodimethylsilyl)phenetole (9.54 g, 0.044 mol), cooled to -65° C., treated dropwise with a 1.3M solution of sec-butyllithium in cyclohexane (34.2 mL, 0.044 mol) while maintaining the temperature below -60° C., stirred at -65° C. for 5 hours, stirred at room temperature overnight, cooled to 0° C., treated with dilute hydrochloric acid, and diluted with ether. The organic phase is separated, washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to obtain a residue which is distilled to give the title product as a clear liquid (7.66 g, bp 84°-92° C./0.8 mm Hg).

1. temperaturewhile maintaining the temperature below -60° C.
2. stirringstirred at room temperature overnight
3. temperaturecooled to 0° C.
4. customThe organic phase is separated
5. washwashed with brine
6. dry with materialdried over anhydrous magnesium sulfate
7. concentrationconcentrated in vacuo
8. customto obtain a residue which
9. distillationis distilled