Sodium Bicarbonate → 8-Bromo-5-chloro-[1,2,4]triazolo[1,5-a]pyridine
반응식
[Br:1][C:2]1[C:3]([NH:9][CH:10]=[N:11]O)=[N:4][C:5]([Cl:8])=[CH:6][CH:7]=1.C([O-])(O)=O.[Na+]>O>[Br:1][C:2]1[C:3]2[N:4]([N:11]=[CH:10][N:9]=2)[C:5]([Cl:8])=[CH:6][CH:7]=1참가 물질
4
실험 절차
N-(3-Bromo-6-chloro-pyridin-2-yl)-N′-hydroxyformamidine (1.62 g, 6.47 mmol) is treated for one hour and 45 minutes with polyphosphoric acid (20 g) at 80° C. After cooling to room temperature, water (200 mL) is added to the reaction mixture. The resulting solution is brought to pH 8 by careful addition of solid NaHCO3 in small portions. The clear solution is extracted three times with dichloromethane. The organic phase is dried over MgSO4, filtered and evaporated. The solid residue (1.44 g) is purified by flash chromatography (silica gel, 4:4:0.7 petroleum ether: dichloromethane: ethyl acetate) to give the title compound (0.75 g) as a solid.
후처리
- extractionThe clear solution is extracted three times with dichloromethane
- dry with materialThe organic phase is dried over MgSO4
- filtrationfiltered
- customevaporated
- customThe solid residue (1.44 g) is purified by flash chromatography (silica gel, 4:4:0.7 petroleum ether: dichloromethane: ethyl acetate)
출처 및 근거
- ORD 기록
- ord-1901673f2742434fa20319fe3e43dd25
- 출처 데이터셋
- uspto-grants-2011_07
- 특허 번호
- US07977352B2
반응 노트
불러오는 중…