Cyclopropylamine → 5-bromo-N-cyclopropylpyridin-2-amine
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5](F)=[N:6][CH:7]=1.[CH:9]1([NH2:12])[CH2:11][CH2:10]1>>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH:12][CH:9]2[CH2:11][CH2:10]2)=[N:6][CH:7]=1参加物
3
反応条件
- 温度
- 80 °C
実験手順
To a sealed tube was added 5-bromo-2-fluoropyridine (1.25 g, 7.10 mmol) and cyclopropylamine (5.0 mL, 72 mmol). Upon heating at 80° C. for 48 hours the reaction was complete. The contents of the tube were transferred to a round bottom flask and concentrated in vacuo. The remaining residue was dissolved in dichloromethane and washed twice with saturated sodium bicarbonate and twice with brine. The organics were dried over sodium sulfate, filtered and concentrated in vacuo to afford the title compound (1.13 g, 75%) as a tan solid.
後処理
- customThe contents of the tube were transferred to a round bottom flask
- concentrationconcentrated in vacuo
- dissolutionThe remaining residue was dissolved in dichloromethane
- washwashed twice with saturated sodium bicarbonate and twice with brine
- dry with materialThe organics were dried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated in vacuo
出典と根拠
- ORDレコード
- ord-2d2e22ead0cd40ed813cf1029e9ffbeb
- 出典データセット
- uspto-grants-2016_01
- 特許番号
- US09227971B2
反応ノート
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