[CH:1]1([C:7]2[CH:28]=[CH:27][C:10]([CH2:11]OP(C3C=CC=CC=3)(C3C=CC=CC=3)=O)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[CH2:29]([Si](C)(C)C)[CH:30]=[CH2:31].C[Si](OS(C(F)(F)F)(=O)=O)(C)C.C(=O)(O)[O-]>COC(OC)C>[CH2:11]([C:10]1[CH:9]=[CH:8][C:7]([CH:1]2[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]2)=[CH:28][CH:27]=1)[CH2:31][CH:30]=[CH2:29]To a stirred mixture of diphenyl-phosphinic acid 4-cyclohexyl-benzyl ester (1 g, 2.56 mmol) and 1.22 ml (7.69 mmol) of allyltrimethylsilane in 12 ml of dry dimethoxy-ethane at 0° C. was added 0.46 ml of trimethylsilyltriflate. The mixture was stirred at 0° C. for 1 h, poured into saturated bicarbonate, extracted with ethyl acetate, washed with water, dried (sodium sulfate) filtered and concentrated. The material was purified by chromatography on silica gel, eluting with ethyl acetate/heptane to provide 0.45 g of the title compound.
読み込み中…
