反应详情

A solution of 2,2'-biphenol (28.1 g, 0.151 mol) in 49 mL phosphorus trichloride was heated at reflux for 2 hr. The excess PC13 was removed by distillation. The residue was purified by vacuum distillation (140°-143° C. at 0.5 mm Hg) to give 30.70 g (81% yield) 1,1'-biphenyl-2,2'-diyl phosphorochloridite (as a clear viscous oil which solidified to a White solid upon standing at room temperature (RT) in an inert atmosphere for an extended period of time). 31P{1H}NMR (121.4 MHz, d8 -toluene): δ180.1 (s), 85% H3PO4 external reference.

1. temperatureat reflux for 2 hr
2. customThe excess PC13 was removed by distillation
3. distillationThe residue was purified by vacuum distillation (140°-143° C. at 0.5 mm Hg)