Aluminium lithium hydride → HCID 59403541、化合物
反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([CH2:13][O:14][C:15]2[CH:26]=[CH:25][C:18]3[C:19](=O)[NH:20][CH2:21][CH2:22][O:23][C:17]=3[CH:16]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C1COCC1>[C:7]1([CH2:13][O:14][C:15]2[CH:26]=[CH:25][C:18]3[CH2:19][NH:20][CH2:21][CH2:22][O:23][C:17]=3[CH:16]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1参加物
4
反応条件
- 温度
- 60 °C
実験手順
1M Lithium aluminium hydride (62.4 ml, 62.4 mmol) in THF was added under argon to a stirred solution of 8-[(phenylmethyl)oxy]-3,4-dihydro-1,4-benzoxazepin-5(2H)-one (Preparation 27) (8.39 g, 31.2 mmol) in THF (150 ml) with ice bath cooling over 5 minutes. The resulting solution was heated with stirring at 60° C. for 3 hours. The reaction was cooled and carefully quenched by slow addition with ice cooling of 150 ml of 2M sodium hydroxide followed by 150 ml of EtOAc. The organics were separated and aqueous extracted with 100 ml of EtOAc. The combined organic extracts were dried (magnesium sulphate) and evaporated to give the title compound (7.53 g) as a light coloured oil. MS (ES) C16H17NO2 requires 255; found 256 [M+H]+.