Aluminium lithium hydride → 2-(3,4-Difluorophenyl)ethanamine
反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([CH:8]=[CH:9][N+:10]([O-])=O)=[CH:4][C:3]=1[F:13].[H-].[Al+3].[Li+].[H-].[H-].[H-]>C1COCC1.CCOCC>[F:13][C:3]1[CH:4]=[C:5]([CH2:8][CH2:9][NH2:10])[CH:6]=[CH:7][C:2]=1[F:1]参加物
5
反応条件
- 温度
- 40 °C
実験手順
To a solution of 1,2-difluoro-4-(2-nitro-vinyl)benzene (1.5 g) in THF (50 mL) is added dropwise lithium aluminum hydride (23 mL, 1M in ether) and the solution is heated at 40° C. for 3 hours. The solution is cooled, diluted with ether and quenched with Na2SO4.10H2O (104 g) overnight. The solid is filtered, and the solution is evaporated in vacuo and chromatographed on silica gel eluting with EtOAc to afford 2-(3,4-difluoro-phenyl)-ethylamine (0.81 g). MS: 170 (M+H); 1H NMR (300 MHz, CDCl3) □6.9-7 (3H, m); 2.95 (2H, t); 2.7 (2H, t).
後処理
- temperatureThe solution is cooled
- customquenched with Na2SO4.10H2O (104 g) overnight
- filtrationThe solid is filtered
- customthe solution is evaporated in vacuo
- customchromatographed on silica gel eluting with EtOAc
出典と根拠
- ORDレコード
- ord-52350acb93e247428b6d89927b833fe4
- 出典データセット
- uspto-grants-2009_04
- 特許番号
- US07517889B2
反応ノート
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