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

HRID 80556

반응식

HRID 80556 반응식
[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

참가 물질

4

반응물 1

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

생성물 1

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

시약·촉매·용매 2

HCID 23925Iron촉매HCID 313Hydrochloric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50a004bff53548748da3cb000baa2d26
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846664B2

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