Water → 2-(Aminomethyl)indole
반응식
[H-].[H-].[H-].[H-].[Li+].[Al+3].[C:7]([C:9]1[NH:10][C:11]2[C:16]([CH:17]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2)#[N:8].O>C1COCC1>[NH2:8][CH2:7][C:9]1[NH:10][C:11]2[C:16]([CH:17]=1)=[CH:15][CH:14]=[CH:13][CH:12]=2참가 물질
5
실험 절차
LAH (42 mL, 1M solution in THF) was added dropwise through a syringe to a solution of 2-cyanoindole (2.0 g, 14.1 mmol) in anhydrous THF (20 mL) with cooling, and the resulting solution was stirred at RT under argon for 5 h. H2O was added dropwise with cooling to destroy excess LAH, and the colorless precipitate was removed by filtration and washed with THF. The filtrate was dried (K2CO3) and concentrated to afford the title compound (2.11 g, quantitative) as a yellow solid: 1H NMR (400 MHz, DMSO-d6) δ 7.41 (d, 1H), 7.29 (d, 1H), 6.97 (t, 1H), 6.91 (t, 1H), 6.20 (s, 1H), 3.82 (s, 2H), 2. 18 (br, 1H).
후처리
- temperaturewith cooling
- temperaturewith cooling
- customto destroy excess LAH
- customthe colorless precipitate was removed by filtration
- washwashed with THF
- dry with materialThe filtrate was dried (K2CO3)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-1c00970b2cd04f03bf78528a187e1121
- 출처 데이터셋
- uspto-grants-1999_11
- 특허 번호
- US05977101
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