HRID1654552

反应详情

EQUATION

反应方程式

HRID 1654552 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

2.44 g (0.02 mol) of 4-hydroxybenzaldehyde, 2.73 g (0.02 mol) of 6-chlorohexanol, 1.66 g (0.012 mol) of potassium carbonate and 20 ml of N,N-dimethylformamide were put in a three-neck 50 ml-flask equipped with a stirrer and a thermometer and heated at 100° C. for 2 hours with stirring. The reaction mixture was cooled to room temperature, poured into water containing ice and extracted with ethyl acetate. The resulting extract was dried with anhydrous sodium sulfate, and ethyl acetate was removed therefrom by distillation. The oily residue was allowed to stand at room temperature, whereupon it gradually crystallized. By silica gel thin layer chromatography (using a developer of ethyl acetate), the purity of the crystals was high. The yield of the product was 4.4 g (99.0%).

WORKUP

后处理

  1. custom50 ml-flask equipped with a stirrer
  2. temperatureThe reaction mixture was cooled to room temperature
  3. additioncontaining ice
  4. extractionextracted with ethyl acetate
  5. extractionThe resulting extract
  6. dry with materialwas dried with anhydrous sodium sulfate, and ethyl acetate
  7. customwas removed
  8. distillationby distillation
  9. customto stand at room temperature, whereupon it
  10. customgradually crystallized