反应详情

As in reaction conditions of Example I, to 3.99 mL of toluene, the 0.04 g of carbonylchlorhydridebis(tricyclohexylphosphine)ruthenium(II) is added and the reaction was carried out between 1.02 g of diethyldivinylgermane and 0.54 g 1-ethynyl-1-(trimethylsiloxy)cyclohexane. Conversion of the terminal alkyne and raw product yield was 65%. In order to remove the catalyst from the system, the solvent and any residual unreacted reactants were evaporated from the post-reaction mixture and the whole material was transferred onto a chromatographic column filled with silica gel modified with a triethylamine, wherafter product was separated, using hexane as eluent. The product, 1-[{diethylvinylgermyl}ethynyl]-1-(trimethylsiloxy)cyclohexane, was obtained at a yield of 55%, in the form of an oily liquid with a light straw color. The product structure was confirmed by 1H, 13C NMR and GCMS analyses.

1. customAs in reaction conditions of Example I
2. customIn order to remove the catalyst from the system
3. customthe solvent and any residual unreacted reactants were evaporated from the post-reaction mixture
4. additionfilled with silica gel
5. customwas separated