関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Trityl chloride | HCID 6456 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 1H-Imidazole-4-carbaldehyde | HCID 76428 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-(triphenylmethyl)-1H-imidazole-4-carbaldehyde | HCID 618233 | — |
反応手順
A solution of trityl chloride (9.5 g, 34.3 mmol) in N,N-dimethylformamide (50 ml) was added dropwise to an ice-cooled solution of imidazole-4-carboxaldehyde (3 g, 31.2 mmol) and triethylamine (17 ml, 125 mmol) in N,N-dimethylformamide (30 ml) and the solution was stirred for 2 hours. The reaction was then allowed to warm to room temperature, and was stirred for a further 18 hours. Water (200 ml) was added, and the resulting pink solid was collected and dried, then dissolved in dichloromethane (200 ml). The resulting solution was washed with water (2×100 ml), dried (MgSO4) and evaporated under reduced pressure. The product was recrystallised from ethanol to afford the title compound as a solid, 7.8 g. 1H-NMR (CDCl3, 400 MHz) δ: 7.06 (m, 6H), 7.32 (m, 9H), 7.48 (s, 1H), 7.58 (s, 1H), 9.82 (s, 1H). Microanalysis found: C, 81.54; H, 5.37; N, 8.24. C23H18N2O requires C, 81.63; H, 5.36; N, 8.28%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06713496B2 |
|---|
| 出典データセット | uspto-grants-2004_03 |
|---|
| ORD ID | ord-7e4a9f9166434d7ba8d06a2ed98ab35d |
|---|
| 出典メモ | uspto-grants-2004_03 |
|---|