4D-083 → HCID 14450229, 화합물
반응식
[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]1참가 물질
3
시약·촉매·용매 1
실험 절차
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.
후처리
- 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
출처 및 근거
- ORD 기록
- ord-7a7fc8ba17e14d108d5fe0783659d6cf
- 출처 데이터셋
- uspto-grants-1983_09
- 특허 번호
- US04404203
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