化工社化工社 化学情報印刷レポート · 研究参考用
(1,1'-Biphenyl)-2,2'-diol → Dibenzo(d,f)(1,3,2)dioxaphosphepin, 6-chloro-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | (1,1'-Biphenyl)-2,2'-diol | HCID 15731 | — |
| 反応物 | Phosphorus trichloride | HCID 24387 | — |
| 生成物 | Dibenzo(d,f)(1,3,2)dioxaphosphepin, 6-chloro- | HCID 612102 | 81% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723641 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-fa67e58f427c410f88c862b2ce6dc73e |
| 出典メモ | uspto-grants-1998_03 |