Water → 2-(Aminomethyl)indole
反応式
[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]=2参加物
5
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-1c00970b2cd04f03bf78528a187e1121
- 出典データセット
- uspto-grants-1999_11
- 特許番号
- US05977101
反応ノート
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