化工社化工社 化学情報印刷レポート · 研究参考用
1-Hydroxybenzotriazole → 9H-carbazole-1-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 9h-Carbazole-1-carboxylic acid | HCID 238924 | — |
| 反応物 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 反応物 | 3-Pyrimidin-5-ylaniline | HCID 7162049 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 9H-carbazole-1-carboxamide | HCID 2058574 | 74.8% |
反応手順
To a suspension of 9H-carbazole-1-carboxylic acid (422 mg) and 1-hydroxybenzotriazole (324 mg) in dichloromethane (10 ml) was added 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (575 mg), and the mixture was stirred for 15 minutes. After adding 3-(pyrimidin-5-yl)aniline (360 mg) and 4-dimethylaminopyridine (367 mg), the mixture was stirred for 48 hours. The residue was evaporated under reduced pressure and purified by a silica gel column chromatography eluting with 2% methanol in dichloromethane to give N-(3-i din-5-yl)-phenyl)-9H-carbazole-1-carboxamide (314 mg, 43.1%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06770667B1 |
| 出典データセット | uspto-grants-2004_08 |
| ORD ID | ord-0dee676d19ee4ec3b5b2ee5737dd97b7 |
| 出典メモ | uspto-grants-2004_08 |