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Acetic Acid → 4-[3-(4-Hydroxy-4-phenyl-piperidin-1-yl)-propyl]-1-(3-trifluoromethyl-phenyl)-[1,4]diazepan-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | 4-Phenylpiperidin-4-ol | HCID 96387 | — |
| 反応物 | Borane;pyridine | HCID 2723995 | — |
| 反応物 | 3-[7-Oxo-4-(3-trifluoromethyl-phenyl)-[1,4]diazepan-1-yl]-propionaldehyde | HCID 86638388 | — |
| 溶媒 | 1,2-Dichloroethane ethanol | HCID 22901612 | — |
| 生成物 | 4-[3-(4-Hydroxy-4-phenyl-piperidin-1-yl)-propyl]-1-(3-trifluoromethyl-phenyl)-[1,4]diazepan-5-one | HCID 59159246 | 44% |
反応手順
To a solution of 3-[7-oxo-4-(3-trifluoromethyl-phenyl)-[1,4]diazepan-1-yl]-propionaldehyde 0.016 g (0.05 mmol) and 4-phenyl-piperidin-4-ol 0.018 g (0.10 mmol) in DCE/EtOH 1:1 (0.5 ml) was added pyridine-borane complex (25 μL of 8 M solution in pyridine, 0.2 mmol) and AcOH (25 μL, 0.4 mmol) and the mixture stirred for 16 h. The mixture was then evaporated to dryness and purified by preparative HPLC, affording the title compound 0.01 g (44%) as a white solid. MS: 476.2 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08138175B2 |
| 出典データセット | uspto-grants-2012_03 |
| ORD ID | ord-08bf37eec1154abcab77aabfd51a5773 |
| 出典メモ | uspto-grants-2012_03 |