2-Amino-5-bromo-4-methyl-3-nitropyridine → 5-bromo-4-methylpyridine-2,3-diamine

HRID 80556

反応式

HRID 80556 の反応式
[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

反応物 1

HCID 72132072-Amino-5-bromo-4-methyl-3-nitropyridine

生成物 1

HCID 101251415-bromo-4-methylpyridine-2,3-diamine

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 313Hydrochloric Acid溶媒

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

  1. temperatureThe reaction was then heated
  2. temperatureto reflux until no starting material
  3. filtrationfiltered
  4. 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

関連ノート

読み込み中…