Oxalic Acid → Pyrido(2,3-b)pyrazine-2,3-diol

HRID 331195ノート

反応式

HRID 331195 の反応式
[NH2:1][C:2]1[C:7]([NH2:8])=[CH:6][CH:5]=[CH:4][N:3]=1.[C:9](O)(=[O:13])[C:10](O)=[O:11]>Cl>[NH:8]1[C:10](=[O:11])[C:9](=[O:13])[NH:1][C:2]2[N:3]=[CH:4][CH:5]=[CH:6][C:7]1=2

参加物

4

反応物 2

HCID 971Oxalic AcidHCID 99562,3-Diaminopyridine

生成物 1

HCID 74947Pyrido(2,3-b)pyrazine-2,3-diol収率 90.1%

試薬・触媒・溶媒 1

HCID 313Hydrochloric Acid溶媒

実験手順

To a suspension of 2,3-diaminopyridine (20 g, 0.136 mol) in 4N aqueous HCl (200 ml) is added oxalic acid (20.7 g, 0.164 mol) and the reaction mixture is refluxed for 20 h. The reaction mixture is cooled and the solid precipitated is filtered, washed with water and dried under vacuum to afford 20 g (89%) of the title compound as a solid. HPLC (max plot) 98%.

後処理

  1. temperaturethe reaction mixture is refluxed for 20 h
  2. temperatureThe reaction mixture is cooled
  3. customthe solid precipitated
  4. filtrationis filtered
  5. washwashed with water
  6. customdried under vacuum

出典と根拠

ORDレコード
ord-190a3110da624507937942cc99b21520
出典データセット
uspto-grants-2014_11
特許番号
US08877757B2

反応ノート

読み込み中…