Multi-step reaction with 4 steps
1: 86 percent / (NH4)2SO4 / 1.) 100 deg C, 5 h; 125 deg C, 19 h, 2.) TMSCl was added to complete conversion at 25 deg C, then 125 deg C, 12 h
2: 1.) n-BuLi, 2.) hexachloroethane / 1.) ether, hexane, 25 deg C, 24 h, 2.) ether, hexane, -40 deg C, 1 h
3: 83 percent / (NH4)2SO4 / 1.) 100 deg C, 5 h; 125 deg C, 19 h, 2.) TMSCl was added to complete conversion at 25 deg C, then 125 deg C, 12 h
4: 1.) n-BuLi, 2.) hexachloroethane / 1.) ether, hexane, 0 deg C, 40 min, 2.) ether, hexane, -40 deg C, 1 h
With
ammonium sulfate; n-butyllithium; hexachloroethane;
DOI:10.1021/ja00195a044