تفاعل #1299

معادلة التفاعل

2,2'-biphenol

phosphorus trichloride

→

1,1'-biphenyl-2,2'-diyl phosphorochloridite

المردود 81.0%

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةat reflux for 2 hr
2. 2
   أخرىThe excess PC13 was removed by distillation
3. 3
   workup.DISTILLATIONThe residue was purified by vacuum distillation (140°-143° C. at 0.5 mm Hg)

الإجراء التجريبي

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.

المصدر