化工社化工社 化学情報印刷レポート · 研究参考用
1,2-Dichloroethane → (4-Azido-phenyl)-(7-methoxy-1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-methanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Azidobenzoic acid | HCID 5325560 | — |
| 反応物 | 7-Methoxy-2,3,4,5-tetrahydro-1h-3-benzazepine | HCID 13853348 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 生成物 | (4-Azido-phenyl)-(7-methoxy-1,2,4,5-tetrahydro-benzo[d]azepin-3-yl)-methanone | HCID 22250962 | — |
反応手順
7-Methoxy-2,3,4,5-tetrahydro-1H-benzo[d]azepine (1 equivalent) was dissolved in THF (0.1 M) along with azidobenzoic acid (1.5 equivalents), EDC (1.5 equivalents), DMAP (0.18 equivalents), and DIEA (1.5 equivalents). The reaction was stirred at room temperature overnight. The reaction was then washed with 10% citric acid, saturated sodium carbonate, and brine. The organic layer was then dried over sodium sulfate and the organic solvent removed under reduced pressure. The material was then purified via flash chromatography using 8% acetone/1% ammonia solution/petroleum spirit running solvent to give the title compound. (MH+) 323.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06995269B2 |
| 出典データセット | uspto-grants-2006_02 |
| ORD ID | ord-934662624998475283d244091759f70e |
| 出典メモ | uspto-grants-2006_02 |