Aluminium lithium hydride → 2-(3,4-Difluorophenyl)ethanamine
반응식
[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]참가 물질
5
반응 조건
- 온도
- 40 °C
실험 절차
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).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-318de45a473a440592e228334f63cd7b
- 출처 데이터셋
- uspto-grants-2012_06
- 특허 번호
- US08193183B2
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