三氟乙酸 → HCID 18615568，化合物
反应方程式
[Br:1][C:2]1[CH:3]=[C:4]([CH:11](O)[CH3:12])[C:5]2[O:9][CH2:8][O:7][C:6]=2[CH:10]=1.FC(F)(F)C(O)=O.C([SiH](CC)CC)C>>[Br:1][C:2]1[CH:3]=[C:4]([CH2:11][CH3:12])[C:5]2[O:9][CH2:8][O:7][C:6]=2[CH:10]=1参与物
4
反应条件
- 温度
- -50 °C
实验过程
To a 250-mL flask was added 1-(6-bromo-benzo[1,3]dioxol4-yl)-ethanol (9.3 g, 37.9 mmol) was added. The solid was cooled to −50° C. and trifluoroacetic acid (44 mL, 568 mmol) was added. Followed addition of triethylsilane (60.5 mL, 379 mmol). The mixture was stirred at reflux for 5 hours, and evaporated in vacuo to an oil. The oil was distilled twice, collecting the fraction boiling between 80° C. and 110° C. at 1.5 mm Hg. The oil was chromatographed on 100 g silica gel, eluted with 5:95 ethyl acetate/hexane. Evaporation of the appropriate fractions gave a clear oil, 6.56 g, 75.6% yield. NMR spectra and elemental analysis were consistent with the structure.