化工社化工社 化学情報印刷レポート · 研究参考用
1,10-Phenanthroline → 4,4'-Dibromo-N,N-diphenyl[1,1'-biphenyl]-2-amine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,10-Phenanthroline | HCID 1318 | — |
| 反応物 | Iodobenzene | HCID 11575 | — |
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 5-Bromo-2-(4-bromophenyl)aniline | HCID 4559420 | — |
| 触媒 | Cuprous chloride | HCID 62652 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 4,4'-Dibromo-N,N-diphenyl[1,1'-biphenyl]-2-amine | HCID 21976317 | 835.7% |
反応手順
4,4′-Dibromo-2-amino-1,1′-biphenyl (16.35 g, prepared according to Libman and Slack (1951) J. Chem. Soc., p. 2588), iodobenzene (26.52 g, 0.13 mol), flake potassium hydroxide (22.4 g, 0.35 mol), 1,10-phenanthroline (0.45 g), copper (I) chloride (0.25 g), and toluene (30 ml) were charged into a flask and stirred at reflux for 15 hours. The dark reaction mixture was cooled to room temperature and diluted with 200 ml of toluene. The toluene solution was washed with DI water, dried with magnesium sulfate, and evaporated. The dark residue obtained was recrystallized trice from hexane/toluene (4:1 volume) to yield 10 grams of white crystals to yield the desired monomer. 1H NMR (CDCl3): δ=6.8–7.5, multiple peaks.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07098297B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-709f53a743134d82ad7ff2bb00604b97 |
| 出典メモ | uspto-grants-2006_08 |