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 | (R)-1-Ethylcarbamoylpiperidine-2-carboxylic acid | HCID 54508361 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | (R)-(1-Methylpiperidin-2-yl)methanol | HCID 853004 | 80% |
反応手順
The product of Step 1 (0.60 g, 0.003 mole) in dry tetrahydrofuran (10 ml) was added dropwise to a suspension of lithium aluminium hydride (0.57 g, 0.015 mole) in dry tetrahydrofuran (20 ml). The mixture was heated under reflux for 2 hours and stirred at room temperature overnight. The reaction mixture was cooled to 0° C. and water (0.5 ml) was added dropwise, followed by 10% sodium hydroxide solution (0.9 ml) and water (1.4 ml). The mixture was stirred for 1 hour, filtered through Celite and the filtrate evaporated in vacuo to afford the title compound 0.31 g (80%) as a pale yellow oil; 1H NMR (CDCl3) 1.17-2.00 (8H, m), 2.14 (1H, dt, J 13 and 2 Hz), 2.30 (3H, s), 2.76-2.96 (1H, m), 3.40 (1H, dd, J 13 and 1 Hz), 3.88 (1H, dd, J 12 and 5 Hz); MS (+ve ion electrospray) m/z 130 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | USRE039128E1 |
|---|
| 出典データセット | uspto-grants-2006_06 |
|---|
| ORD ID | ord-d3603aaa52494c6088368e879a2c239f |
|---|
| 出典メモ | uspto-grants-2006_06 |
|---|