Hydrazine hydrate (1:1) → 1-(5-Bromo-4-methylpyridin-2-YL)hydrazine
反応式
[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5](Cl)=[N:6][CH:7]=1.O.[NH2:11][NH2:12]>CCO>[Br:1][C:2]1[C:3]([CH3:9])=[CH:4][C:5]([NH:11][NH2:12])=[N:6][CH:7]=1参加物
4
反応条件
- 温度
- 120 °C
実験手順
Combined 5-bromo-2-chloro-4-methylpyridine (15.0 g, 72.46 mmol) and EtOH (60 mL) and added hydrazine hydrate (85%, 45 mL) and stirred at 120° C. overnight. The reaction mixture was concentrated to give a residue which was extracted with EtOAc (50 mL×2) and water (50 mL×2). Then combined organic layers were extracted with brine, dried over Na2SO4 to and concentrated to give a residue which was purified by flash chromatography (petroleum ether:EtOAc=10:1 to 1:5) to give the title compound (7.8 g, 53%).
後処理
- concentrationThe reaction mixture was concentrated
- customto give a residue which
- extractionwas extracted with EtOAc (50 mL×2) and water (50 mL×2)
- extractionThen combined organic layers were extracted with brine
- dry with materialdried over Na2SO4 to and
- concentrationconcentrated
- customto give a residue which
- customwas purified by flash chromatography (petroleum ether:EtOAc=10:1 to 1:5)
出典と根拠
- ORDレコード
- ord-7da27c81cd8c49378b166f582c0762f6
- 出典データセット
- uspto-grants-2015_05
- 特許番号
- US09040522B2
反応ノート
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