Ethanol → 5-Bromo-N-methyl-3-nitropyridin-2-amine

HRID 445621

反応式

HRID 445621 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[CH3:12][NH2:13].CCO>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([N+:9]([O-:11])=[O:10])[C:5]([NH:13][CH3:12])=[N:6][CH:7]=1

参加物

5

反応物 3

HCID 702EthanolHCID 6329MethylamineHCID 70194125-Bromo-2-chloro-3-nitropyridine

生成物 1

HCID 108681495-Bromo-N-methyl-3-nitropyridin-2-amine

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of 5-bromo-2-chloro-3-nitropyridine (Matrix, Columbia, USA, 9.8 g, 41.3 mmol) in 250 ml THF was added 8 M methylamine in EtOH (Aldrich, Buchs, Switzerland, 12.9 ml, 103 mmol). The reaction mixture was stirred 1 h at rt then was quenched with 300 ml water. The precipite was filtered and the filtrate concentrated before being filtered again. The yellow solids were combined and dried to give the title compound as a yellow solid (HPLC: tR 3.13 min (Method A)).

後処理

  1. customthen was quenched with 300 ml water
  2. filtrationThe precipite was filtered
  3. concentrationthe filtrate concentrated
  4. filtrationbefore being filtered again
  5. customdried

出典と根拠

ORDレコード
ord-a355d5361bce4509af81f3ec9290f393
出典データセット
uspto-grants-2013_07
特許番号
US08476294B2

関連ノート

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