化工社化工社 化学情報印刷レポート · 研究参考用
9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one → 9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one | HCID 20522041 | — |
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | 9-Benzyl-1-oxa-4,9-diazaspiro[5.5]undecane | HCID 35753744 | 82.7% |
反応手順
To a stirring mixture of lithium aluminum hydride (2.22 g, 58.5 mmol) in tetrahydrofuran (70 mL) was added compound 399 (3.60 g, 13.8 mmol), portionwise over three minutes. After 1.25 hours of reflux the reaction was cooled to room temperature and quenched with water (2.22 mL), then 1N NaOH (2.22 mL), then water (2×2.22 mL). The remaining solids were filtered off, and the filtrate was concentrated to give compound 402 (2.81 g, 82%). LCMS-ESI (POS), M/Z, M+1: Found 247.1, Calculated 247.2.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08980903B2 |
| 出典データセット | uspto-grants-2015_03 |
| ORD ID | ord-2dcc43ea69014a0ebf47a4682f6e2514 |
| 出典メモ | uspto-grants-2015_03 |