(1,1'-Biphenyl)-2,2'-diol → Dibenzo(d,f)(1,3,2)dioxaphosphepin, 6-chloro-

HRID 1203

반응식

HRID 1203 반응식
[C:1]1([OH:14])[C:2]([C:7]2[C:8]([OH:13])=[CH:9][CH:10]=[CH:11][CH:12]=2)=[CH:3][CH:4]=[CH:5][CH:6]=1.[P:15](Cl)(Cl)[Cl:16]>>[P:15]1([Cl:16])[O:13][C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][C:7]=2[C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][C:1]=2[O:14]1

참가 물질

3

반응물 2

HCID 15731(1,1'-Biphenyl)-2,2'-diolHCID 24387Phosphorus trichloride

생성물 1

HCID 612102Dibenzo(d,f)(1,3,2)dioxaphosphepin, 6-chloro-수율 81%

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-fa67e58f427c410f88c862b2ce6dc73e
출처 데이터셋
uspto-grants-1998_03
특허 번호
US05723641

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