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Diisopropylethylamine → 1-(trans-3-(4-Chlorophenyl)allyl)-perhydroazepin-4-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | Azepan-4-one hydrochloride | HCID 22021728 | — |
| 反応物 | p-Chlorocinnamyl chloride | HCID 53728250 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 1-(trans-3-(4-Chlorophenyl)allyl)-perhydroazepin-4-one | HCID 68927305 | 48.3% |
反応手順
4-Perhydroazepinone hydrochloride (2.5 g, prepared according to Synth. Commun. 1992, 1249-1258) was suspended in acetonitrile (80 ml); diisopropylethylamine (4.4 ml) and 4-chlorocinnamyl chloride (2.7 g) were successively added at room temperature and the resulting reaction mixture was stirred at room temperature for 20 hours. The solvent was removed in vacuo and the residue purified by silica gel chromatography (eluent cyclohexane:ethyl acetate 6:4) to afford 1-(trans-3-(4-chlorophenyl)allyl)-perhydroazepin-4-one (1.84 g) as a foam. MS (ES+) 264/266 (M+H+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08846907B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-ca98a52b02d141e9a3692979e8c3ee85 |
| 出典メモ | uspto-grants-2014_09 |