Aluminium lithium hydride → HCID 86719159、化合物
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]([O:11][C:12](=[O:21])[NH:13][C@@H:14]([C:16](=O)[N:17]([CH3:19])[CH3:18])[CH3:15])([CH3:10])([CH3:9])[CH3:8]>CCOCC>[C:7]([O:11][C:12](=[O:21])[NH:13][C@H:14]([CH3:15])[CH2:16][N:17]([CH3:18])[CH3:19])([CH3:10])([CH3:9])[CH3:8]参加物
4
反応条件
- 温度
- 0 °C
実験手順
Reduction was carried out according to Chem. Eur. J. (2008), 14(17), 51116-5119. To an ice-cooled lithium aluminum hydride (in Et2O) (21.35 mL, 21.35 mmol) solution was added drop wise a solution of ((R)-1-dimethylcarbamoyl-ethyl)-carbamic acid tert-butyl ester (1.7105 g, 7.12 mmol) in Et2O (2-3 mL). The reaction mixture was stirred at 0° C. until disappearance of the starting material. The reaction mixture was carefully quenched by sequential addition of water (1.2 mL), 15% (w/w) NaOH (1.2 mL) and water (3.6 mL). Then EtOAc was added and the solids were filtered and washed with EtOAc. The filtrated was dried over MgSO4, filtered and evaporated off. Then the crude was dissolved in DCM, filtered and evaporated off to give 1.4543 g, 6.47 mmol, 91% yield ((R)-2-Dimethylamino-1-methyl-ethyl)-carbamic acid tert-butyl ester as yellowish oil. The crude was used without any further purification and characterization.