化工社化工社 化学情報印刷レポート · 研究参考用
Triphenylphosphine → 2,7-difluoro-9H-carbazole
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triphenylphosphine | HCID 11776 | — |
| 反応物 | 4,4'-Difluoro-2-nitro-1,1'-biphenyl | HCID 345411 | — |
| 溶媒 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 生成物 | 2,7-difluoro-9H-carbazole | HCID 59326141 | 82% |
反応手順
A solution of 4,4′-difluoro-2-nitro-1,1′-biphenyl (0.580 g, 2.5 mmol) and triphenylphosphine (1.617 g, 6.2 mmol) in anhydrous 1,2-dichlorobenzene (5 mL) was heated to 175° C. in a microwave reactor for 4 hrs. The mixture was cooled to room temperature and concentrated to a black residue under high vacuum. The crude product was purified by silica gel chromatography (5-50% methylene chloride/hexanes) to afford the product as a light brown powder (0.41 g, 82%). 1H NMR (CDCl3, 300 MHz) δ 8.10 (br s, 1H), 7.93 (dd, 2H, J=8.7, 5.4 Hz), 7.11 (dd, 2H, J=9.3, 2.4 Hz), 6.99 (ddd, 2H, J=9.6, 9.0, 2.4 Hz).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09265772B2 |
| 出典データセット | uspto-grants-2016_02 |
| ORD ID | ord-3b6fc24c887b4cd6a2171eeef7d61b57 |
| 出典メモ | uspto-grants-2016_02 |