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Triphenylphosphine dibromide → 4-Bromo-4'-(bromomethyl)-1,1'-biphenyl
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine dibromide | HCID 70579 | — |
| 反応物 | [4-(4-Bromophenyl)phenyl]methanol | HCID 1393673 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Bromo-4'-(bromomethyl)-1,1'-biphenyl | HCID 20137344 | — |
反応手順
A solution of (4′-bromo-biphenyl-4-yl)-methanol, 7.01 g (27.9 mmol) and dibromo-triphenylphosphorane 11.8 g (27.9 mmol) in 150 mL of methylene chloride stirred at room temperature for 2 h. The solution was diluted with 100 mL of water and extracted with 2×200 mL portions of diethyl ether. The organic layers were combined, washed with sat. aq. NaCl, and dried (MgSO4). After the solution was concentrated, the residue was purified through a short plug of silica gel (eluted with 50% EtOAc-Heptane) to afford the desired product in 9.1 g (100%) as a white solid. The material was taken to the next step without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07498356B2 |
| 出典データセット | uspto-grants-2009_03 |
| ORD ID | ord-6b21c13c0f3b44b3bddb7e6cd4e61e8f |
| 出典メモ | uspto-grants-2009_03 |