Aluminium lithium hydride → 3-(2-Aminoethyl)-N-benzyloxetan-3-amine
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([NH:14][C:15]1([CH2:19][C:20]#[N:21])[CH2:18][O:17][CH2:16]1)[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1>C(OCC)C>[NH2:21][CH2:20][CH2:19][C:15]1([NH:14][CH2:7][C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:18][O:17][CH2:16]1参加物
4
反応条件
- 温度
- 0 °C
実験手順
To a cooled slurry of lithium aluminium hydride (327 mg, 8.6 mmol) in anhydrous diethyl ether (40 mL), was added a solution of 3-(benzylamino)oxetan-3-acetonitrile (1.0 g, 4.3 mmol) in anhydrous diethyl ether (10 mL) dropwise at 0° C. After being stirred at 0° C. for 2 hours, the reaction was quenched by introducing disodium sulfate decahydrate slowly. After being stirred for 30 minutes, the mixture was filtered, and the filter cake was washed with ethyl acetate. The filtrate was dried over sodium sulfate and concentrated in vacuo. The residue was purified by flash column to afford 800 mg of 3-(aminoethyl)-N-benzyloxetan-3-amine as a light yellow oil (yield was 79%).