HRID1976051
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
To phosphorous oxychloride (2.02 ml, 21.6 mmol) was added quinoline (1.34 ml, 11.2 mmol) followed by 3-bromo-2-hydroxy-5-trifluoromethylpyridine (5.0 g, 20.7 mmol), and the mixture formed heated at 120° C. for 3 hrs. It was then cooled to 100° C. and water (10 ml) added. After cooling to 22° C., sodium hydrogen carbonate solution (100 ml) was added and the mixture extracted with ethyl acetate (2×100 ml). The extracts were dried (MgSO4) and concentrated, and the residue purified by silica chromatography to give the product as an oil (4.05 g, 75% yield).
WORKUP
后处理
- customthe mixture formed
- temperatureIt was then cooled to 100° C.
- temperatureAfter cooling to 22° C.
- extractionthe mixture extracted with ethyl acetate (2×100 ml)
- dry with materialThe extracts were dried (MgSO4)
- concentrationconcentrated
- customthe residue purified by silica chromatography