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Aluminium lithium hydride → Trv-0109662
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aluminium lithium hydride | HCID 21226445 | — |
| 反応物 | (R)-2-(9-(Pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl)acetonitrile | HCID 68314099 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | Trv-0109662 | HCID 68314401 | 94% |
反応手順
LAH (1M in Et2O, 20 ml, 20 mmol) was added to a solution of 2-[(9R)-9-(pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]acetonitrile (2.56 g, 10 mmol) in Et2O (100 ml, 0.1M) at 0° C. under N2. The resulting mix was stirred and allowed to warm to room temperature. After 2 h, LCMS showed the reaction had completed. The reaction was cooled at 0° C. and quenched with water (1.12 ml), NaOH (10%, 2.24 ml) and another 3.36 ml of water. Solid was filtered and filter pad was washed with ether (3×20 ml). The combined organic was dried and concentrated to give 2-[(9R)-9-(Pyridin-2-yl)-6-oxaspiro[4.5]decan-9-yl]ethan-1-amine (2.44 g, 94% yield, m/z 260.6 [M+H]+ observed) as a light amber oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09044469B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-7d99ca31b0324fe1bf6406180db7acf3 |
| 出典メモ | uspto-grants-2015_06 |