反应详情

Triethylsilane (7.0 g) is added dropwise over 2 h to a cooled, stirred (0° C.) solution of 1E (8.0 g) in trifluoroacetic acid (40 ml). The reaction mixture is stirred at room temperature overnight and poured into NaHCO3 solution. The product is extracted into ether twice and the combined ether layers are washed with water and dried (MgSO4). The solvent was removed in vacuo to yield an orange-brown oil. The crude product is distilled under reduced pressure (short path, 110°-120° C. at 0.01 mm Hg) to give a red oil.

1. extractionThe product is extracted into ether twice
2. washthe combined ether layers are washed with water
3. dry with materialdried (MgSO4)
4. customThe solvent was removed in vacuo
5. customto yield an orange-brown oil
6. distillationThe crude product is distilled under reduced pressure (short path, 110°-120° C. at 0.01 mm Hg)
7. customto give a red oil