Oxalic Acid → 6-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione

HRID 1488977노트

반응식

HRID 1488977 반응식
[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:13]=[CH:12][C:11]([NH2:14])=[C:10]([NH2:15])[CH:9]=2)[CH:4]=[CH:3]1.[C:16](O)(=[O:20])[C:17](O)=[O:18]>Cl>[O:1]=[C:2]1[CH:7]=[CH:6][N:5]([C:8]2[CH:9]=[C:10]3[C:11](=[CH:12][CH:13]=2)[NH:14][C:17](=[O:18])[C:16](=[O:20])[NH:15]3)[CH:4]=[CH:3]1

참가 물질

4

반응물 2

HCID 971Oxalic AcidHCID 229035884-(4-Oxo-4H-pyridin-1-yl)-1,2-phenylenediamine

생성물 1

HCID 229035916-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione수율 77.8%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

실험 절차

First, 4.849 g of 4-(4-oxo-4H-pyridin-1-yl)-1,2-phenylenediamine and 2.402 g of oxalic acid were added to 60 ml of 4N hydrochloric acid. The mixture was refluxed by heating for 2.5 hours in a nitrogen atmosphere. After the mixture was cooled, precipitated crystals were filtered and recrystallized with dimethylformamide to give 4.786 g of 6-(4-oxo-4H-pyridin-1-yl)-1,4-dihydroquinoxaline-2,3-dione.

후처리

  1. temperatureThe mixture was refluxed
  2. temperatureby heating for 2.5 hours in a nitrogen atmosphere
  3. temperatureAfter the mixture was cooled
  4. customprecipitated crystals
  5. filtrationwere filtered
  6. customrecrystallized with dimethylformamide

출처 및 근거

ORD 기록
ord-f6d3b3a5c0154007b754295d8408d2cd
출처 데이터셋
uspto-grants-1997_10
특허 번호
US05677305

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