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

HRID 655622ノート

反応式

HRID 655622 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-44595e1950244a75944f176da37f0f04
出典データセット
uspto-grants-2011_12
特許番号
US08071597B2

反応ノート

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