2-Amino-5-bromo-4-methyl-3-nitropyridine → 5-Bromo-4-methylpyridine-2,3-diamine
反応式
[NH2:1][C:2]1[C:7]([N+:8]([O-])=O)=[C:6]([CH3:11])[C:5]([Br:12])=[CH:4][N:3]=1>Cl.[Fe]>[Br:12][C:5]1[C:6]([CH3:11])=[C:7]([NH2:8])[C:2]([NH2:1])=[N:3][CH:4]=1参加物
4
実験手順
2-Amino-5-bromo-4-methyl-3-nitropyridine (5 g) was dissolved in 6M HCl (50 mL) and iron powder was slowly added. The reaction was then heated to reflux until no starting material was seen via HPLC. The reaction was then cooled to room temperature and filtered. The bis-HCl salt was dried to a cream solid which was then taken up in EtOAc, neutralized with 50% NaOH solution to yield 5-bromo-4-methylpyridine-2,3-diamine as a free base.
後処理
- temperatureThe reaction was then heated
- temperatureto reflux until no starting material
- filtrationfiltered
- dry with materialThe bis-HCl salt was dried to a cream solid which
出典と根拠
- ORDレコード
- ord-50a004bff53548748da3cb000baa2d26
- 出典データセット
- uspto-grants-2014_09
- 特許番号
- US08846664B2
反応ノート
読み込み中…