Sodium Bicarbonate → 8-Bromo-5-chloro-[1,2,4]triazolo[1,5-a]pyridine
反応式
[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]=1参加物
4
実験手順
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.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-1901673f2742434fa20319fe3e43dd25
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07977352B2
反応ノート
読み込み中…