4D-083 → HCID 14450229、化合物
反応式
[O:1]=[C:2]1[C:7]([C:8]([NH2:10])=O)=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1>C(OC(=O)C)(=O)C>[O:1]=[C:2]1[C:7]([C:8]#[N:10])=[CH:6][C:5]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[N:4][NH:3]1参加物
3
試薬・触媒・溶媒 1
実験手順
A mixture of 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarboxamide (4.2 g) in 100 ml of acetic anhydride is heated under reflux for 6 hours. The acetic anhydride is removed by distillation and the residue is partitioned between ammonium hydroxide solution and dichloromethane. The dichloromethane layer is separated and concentrated on the rotary evaporator and the residue is recrystallized from ethanol to give 2,3-dihydro-3-oxo-6-phenyl-4-pyridazinecarbonitrile.
後処理
- temperatureis heated
- temperatureunder reflux for 6 hours
- customThe acetic anhydride is removed by distillation
- customthe residue is partitioned between ammonium hydroxide solution and dichloromethane
- customThe dichloromethane layer is separated
- concentrationconcentrated on the rotary evaporator
- customthe residue is recrystallized from ethanol
出典と根拠
- ORDレコード
- ord-7a7fc8ba17e14d108d5fe0783659d6cf
- 出典データセット
- uspto-grants-1983_09
- 特許番号
- US04404203
反応ノート
読み込み中…