Hydrochloric Acid → 3-Amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxylic acid

HRID 915025ノート

反応式

HRID 915025 の反応式
[NH2:1][C:2]1[C:3]([C:24](N)=[O:25])=[N:4][C:5]([C:14]2[CH:19]=[CH:18][C:17](=[O:20])[N:16]([CH:21]([CH3:23])[CH3:22])[N:15]=2)=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:7]=1.Cl.[OH-:28].[Na+]>O1CCOCC1>[NH2:1][C:2]1[C:3]([C:24]([OH:25])=[O:28])=[N:4][C:5]([C:14]2[CH:19]=[CH:18][C:17](=[O:20])[N:16]([CH:21]([CH3:23])[CH3:22])[N:15]=2)=[C:6]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:7]=1

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 116532023-Amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide

生成物 1

HCID 693332313-Amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxylic acid

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
92.5 °C

実験手順

A suspension of 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxamide (1.02 g) in a mixture of conc. HCl (40 ml) and dioxane (10 ml) was heated at 90-95° C. for 20 hours. Under ice-cooling, the reaction mixture was adjusted to pH 4 with 4N aq. NaOH solution to yield a precipitate. The precipitate was collected by filtration and dried at 60° C. under reduced pressure to give 3-amino-6-(1-isopropyl-6-oxo-1,6-dihydro-3-pyridazinyl)-5-phenyl-2-pyrazinecarboxylic acid as a solid (878 mg).

後処理

  1. temperatureUnder ice-cooling
  2. customto yield a precipitate
  3. filtrationThe precipitate was collected by filtration
  4. customdried at 60° C. under reduced pressure

出典と根拠

ORDレコード
ord-64ab9dbaf41742f9befe6e6f051b7006
出典データセット
uspto-grants-2007_09
特許番号
US07265120B2

反応ノート

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