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 | N-(1-adamantylmethyl)-5-methyl-3-oxohexanamide | HCID 59437162 | — |
| 溶媒 | Tetrahydrofuran | HCID 8028 | — |
| 生成物 | HCID 59437180 | HCID 59437180 | 63.3% |
反応手順
A solution of N-(1-adamantylmethyl)-5-methyl-3-oxohexanamide (1.5 g, 5.1 mmol) in anhydrous THF (15 mL) was added slowly to a suspension of LAH (500 mg, 13.1 mmol) in anhydrous THF (5 mL) under N2 at 0° C. The reaction mixture was heated to 70° C. and stirred at this temperature overnight. Water (0.5 mL) and 10% aq NaOH (0.5 mL) were added to quench the reaction. The resulting slurry was filtered. The filtrate was concentrated in vacuo and the residue was purified by chromatography on a silica gel column eluted with 10:1 PE/EtOAc to give 1-(1-adamantylmethylamino)-5-methylhexan-3-ol (900 mg, 63.3%). MS (M+1): 280.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08835426B2 |
|---|
| 出典データセット | uspto-grants-2014_09 |
|---|
| ORD ID | ord-3a0ef8e6fb3944ec947316a942c21f3d |
|---|
| 出典メモ | uspto-grants-2014_09 |
|---|
