6-Bromo-3-methoxy-2-nitropyridine → 2-Amino-6-bromo-3-methoxypyridine

HRID 1772884ノート

反応式

HRID 1772884 の反応式
[Br:1][C:2]1[N:7]=[C:6]([N+:8]([O-])=O)[C:5]([O:11][CH3:12])=[CH:4][CH:3]=1>[Fe].CC(O)=O>[Br:1][C:2]1[N:7]=[C:6]([NH2:8])[C:5]([O:11][CH3:12])=[CH:4][CH:3]=1

参加物

4

反応物 1

HCID 226151626-Bromo-3-methoxy-2-nitropyridine

生成物 1

HCID 575629062-Amino-6-bromo-3-methoxypyridine収率 81.2%

試薬・触媒・溶媒 2

HCID 23925Iron触媒HCID 176Acetic Acid溶媒

反応条件

温度
90 °C

実験手順

A mixture of 6-bromo-3-methoxy-2-nitropyridine (14.4 g, 61.8 mmol), AcOH (200 mL) and Fe powder (14.0 g, 0.25 mol) was stirred at 90° C. for 1.5 h. After cooling to rt and dilution with EtOAc the mixture was filtered through celite and the filtrate concentrated in vacuo. Purification by flash chromatography eluting with DCM yielded the title compound (10.2 g, 50.2 mmol) as a white solid.

後処理

  1. temperatureAfter cooling to rt
  2. filtrationdilution with EtOAc the mixture was filtered through celite
  3. concentrationthe filtrate concentrated in vacuo
  4. customPurification by flash chromatography
  5. washeluting with DCM

出典と根拠

ORDレコード
ord-796c49612d6244109b8cd94804124d62
出典データセット
uspto-grants-2016_02
特許番号
US09249160B2

反応ノート

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