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
PROCEDURE
实验过程
5.5 g of 2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldoxime and 4.6 g of 3-chlorocinnamyl bromide were dissolved in 30 ml of dry acetone containing 2.7 g of anhydrous potassium carbonate. The solution was heated for 5 hours under stirring and reflux. After the reaction mixture was allowed to cool down, the acetone was distilled out under reduced pressure and the resulting residue was dissolved in 200 ml of ethyl acetate. The ethyl acetate solution was washed with water and the organic layer was dried over anhydrous sodium sulfate. The solution was then concentrated under reduced pressure. The residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate:4:1) to obtain 5.2 g of 0-(3-chlorocinnamyl)-2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldoxime as a semi-solid substance.
WORKUP
后处理
- temperatureThe solution was heated for 5 hours
- temperaturereflux
- temperatureto cool down
- distillationthe acetone was distilled out under reduced pressure
- dissolutionthe resulting residue was dissolved in 200 ml of ethyl acetate
- washThe ethyl acetate solution was washed with water
- dry with materialthe organic layer was dried over anhydrous sodium sulfate
- concentrationThe solution was then concentrated under reduced pressure
- customThe residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate:4:1)