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1,2-Dichloroethane → 1-[4-(5,6,7,8-Tetrahydro-1H-pyrrolo[3,2-b]azepine-4-carbonyl)piperidin-1-yl]-ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1,2-Dichloroethane | HCID 11 | — |
| 反応物 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 反応物 | 1-Acetylpiperidine-4-carboxylic acid | HCID 117255 | — |
| 反応物 | 1,4,5,6,7,8-Hexahydropyrrolo[3,2-B]azepine | HCID 22561790 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-[4-(5,6,7,8-Tetrahydro-1H-pyrrolo[3,2-b]azepine-4-carbonyl)piperidin-1-yl]-ethanone | HCID 22561858 | 95% |
反応手順
To a mixture of 1-acetyl-piperidine-4-carboxylic acid (822 mg, 4.8 mmol, 1.2 eq.), EDC (920 mg, 1.2 eq.), HOBt (648 mg, 1.2 eq.) in DCM (15 mL) was added TEA (1.3 mL, 2 eq.) and 1,4,5,6,7,8-hexahydro-pyrrolo[3,2-b]azepine (550 mg, 4 mmol). The mixture was stirred at rt for 2 days. The reaction was diluted with DCM, washed with water, sat. NaHCO3, brine, dried and concentrated. The residue was purified on a silica gel column to give 1.1 g of 1-[4-(5,6,7,8-tetrahydro-1H-pyrrolo[3,2-b]azepine-4-carbonyl)-piperidin-1-yl]-ethanone as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06861418B2 |
| 出典データセット | uspto-grants-2005_03 |
| ORD ID | ord-6632b5eaed124fabb2dbfa3e4ac8df1b |
| 出典メモ | uspto-grants-2005_03 |