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

HRID 227755

反応式

HRID 227755 の反応式
[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

参加物

4

反応物 3

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

生成物 1

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

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-2fc91df96b494e9cb0b925390975d41c
出典データセット
uspto-grants-2009_07
特許番号
US07560551B2

関連ノート

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