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Water → 1-benzyl-N-trityl-3-azepanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | 1-Benzyl-3-(tritylamino)-2-azepanone | HCID 69431014 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 1-benzyl-N-trityl-3-azepanamine | HCID 69428688 | 78% |
反応手順
A solution of 1-benzyl-3-(tritylamino)-2-azepanone (425 mg, 0.922 mmol) in tetrahydrofuran (11 ml) was added dropwise to a suspension of lithium aluminum hydride (140 mg, 3.69 mmol) in tetrahydrofuran (22 ml) at room temperature, and the resulting mixture was stirred for 30 minutes and then refluxed for 3 hours. After the reaction mixture was cooled, water (0.14 ml), a 2N-aqueous sodium hydroxide solution (0.3 ml) and water (0.14 ml) were added thereto under ice-cooling. The resulting mixture was filtered and the solvent of the filtrate was distilled off under reduced pressure. The resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol) to obtain 1-benzyl-N-trityl-3-azepanamine (319 mg, 78%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07199147B2 |
| 出典データセット | uspto-grants-2007_04 |
| ORD ID | ord-70e29d5b765a4080a3334b3c37b41b53 |
| 出典メモ | uspto-grants-2007_04 |