反应详情

温度

150 °C

A mixture of 20 g. of 5-methylene-4-triethylsilyloxy-1-octyne, 25.36 g. of tri-n-butylstannane and 0.1 g. of azobisisobutyrylnitrile is placed in an oil bath at 100° C. After 10 minutes an exotherm raises the temperature to 150° C. The mixture is then heated at 130°-140° C. for 1.5 hours. The excess tri-n-butylstannane is distilled off at 130° C. (1 mm.) and the residue is distilled in a Kugelrohr at 120°-140° C., 0.15-0.05 mm., giving the product as a colorless liquid.

1. additionA mixture of 20 g
2. temperatureThe mixture is then heated at 130°-140° C. for 1.5 hours
3. distillationThe excess tri-n-butylstannane is distilled off at 130° C. (1 mm.)
4. distillationthe residue is distilled in a Kugelrohr at 120°-140° C.