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

HRID 331195노트

반응식

HRID 331195 반응식
[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

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 99562,3-Diaminopyridine

생성물 1

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

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-190a3110da624507937942cc99b21520
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877757B2

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