Phosphorus oxychloride → 3-(3-Bromo-4-methoxyphenyl)-6-chloropyridazine
반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:10]2[CH:11]=[CH:12][C:13](=O)[NH:14][N:15]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].P(Cl)(Cl)([Cl:19])=O>>[Br:1][C:2]1[CH:3]=[C:4]([C:10]2[N:15]=[N:14][C:13]([Cl:19])=[CH:12][CH:11]=2)[CH:5]=[CH:6][C:7]=1[O:8][CH3:9]참가 물질
3
실험 절차
A suspension of 100 g. of 6-(3-bromo-4-methoxyphenyl)-3(2H)-pyridazinone [J. Heterocyclic Chem. 11, 775 (1974) ]in 150 ml. of phosphorus oxychloride is refluxed until a clear solution is obtained (approximately 5 hours). The solution is cooled and excess phosphorus oxychloride is removed under vacuum to give a brown solid which is triturated with ice water. The solid is collected by filtration and is recrystallized to afford 3-(3-bromo-4-methoxyphenyl)-6-chloropyridazine.
후처리
- additionA suspension of 100 g
- customis obtained (approximately 5 hours)
- temperatureThe solution is cooled
- customexcess phosphorus oxychloride is removed under vacuum
- customto give a brown solid which
- customis triturated with ice water
- filtrationThe solid is collected by filtration
- customis recrystallized
출처 및 근거
- ORD 기록
- ord-262367b5719642fcbfb863d0973c56b2
- 출처 데이터셋
- uspto-grants-1978_09
- 특허 번호
- US04112095
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