HRID344573

反应详情

EQUATION

反应方程式

HRID 344573 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5.5 g of 2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldoxime and 4.2 g of 3-methylcinnamyl bromide were dissolved in 30 ml of acetonitrile containing 2.7 g of anhydrous potassium carbonate, and the solution was heated for 5 hours under stirring and reflux. After the reaction mixture was allowed to cool down, the acetonitrile 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-methylcinnamyl)-2-(4,6-dimethoxy-2-pyrimidinyloxy)benzaldoxime as crystals.

WORKUP

后处理

  1. temperaturethe solution was heated for 5 hours
  2. temperaturereflux
  3. temperatureto cool down
  4. distillationthe acetonitrile was distilled out under reduced pressure
  5. dissolutionthe resulting residue was dissolved in 200 ml of ethyl acetate
  6. washThe ethyl acetate solution was washed with water
  7. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  8. concentrationThe solution was then concentrated under reduced pressure
  9. customThe residue was purified by silica gel chromatography (developer: n-hexane:ethyl acetate:4:1)