Acetic Acid → 5H,6H,7H,8H-pyrazino(2,3-d)pyridazine-5,8-dione

HRID 593930노트

반응식

HRID 593930 반응식
[N:1]1[CH:6]=[CH:5][N:4]=[C:3]2[C:7]([O:9][C:10](=[O:11])[C:2]=12)=O.O.[NH2:13][NH2:14].C(O)(=O)C>>[N:1]1[C:2]2[C:10](=[O:11])[NH:13][NH:14][C:7](=[O:9])[C:3]=2[N:4]=[CH:5][CH:6]=1

참가 물질

4

반응물 3

HCID 176Acetic AcidHCID 24654Hydrazine hydrate (1:1)HCID 78482Furo(3,4-b)pyrazine-5,7-dione

생성물 1

HCID 8197895H,6H,7H,8H-pyrazino(2,3-d)pyridazine-5,8-dione

실험 절차

The title compound was prepared according to a literature procedure (Paul, D. B. Aust. J. Chem. 1974, 27, 1331). As described therein, 2,3-pyrazinedicarboxylic anhydride (5.00 g, 33.3 mmol), hydrazine hydrate (2.8 g, 56 mmol), and acetic acid (40.4 ml, 33.3 mmol) were mixed at RT. White precipitated crashed out. The reaction was heated under reflux for approximately 20 min. The reaction was cooled to RT and the solids were filtered, washed with water, and dried under vacuum. The product, 6,7-dihydropyrazino[2,3-d]pyridazine-5,8-dione was obtained as white solid. 1H NMR (Bruker, 400 MHz, D2O) ppm: 8.87 (s, 2H).

후처리

  1. customThe title compound was prepared
  2. customWhite precipitated
  3. temperatureThe reaction was heated
  4. temperatureunder reflux for approximately 20 min
  5. filtrationthe solids were filtered
  6. washwashed with water
  7. customdried under vacuum

출처 및 근거

ORD 기록
ord-6d84b4a261224c8e9a0c46ef87e33e66
출처 데이터셋
uspto-grants-2016_01
특허 번호
US09242961B2

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