HRID2246021

反应详情

EQUATION

反应方程式

HRID 2246021 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.80 g (4.6 mmol) bis[6-chlorohexyl]2,2 bis(4-nitrobenzyl)malonate, 3.0 g (9.2 mmol) 4-pentoxyphenyl (2E)-3-{4-hydroxyphenyl}acrylate and 0.17 g (0.46 mmol) tetrabutylammonium iodide were dissolved in 30 ml 2-butanone. 2.53 g (18.3 mmol) potassium carbonate were added. The resulting suspension was heated at refluxing temperature and allowed to react for 48 h. After cooling to room temperature, the reaction mixture was partitioned between ethyl acetate and water. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation to yield 3.6 g bis[6-{4-[(1E)-3-(4-pentyloxyphenoxy)-3-oxoprop-1-enyl]phenoxy}hexyl]2,2 bis(4-nitrobenzyl)malonate.

WORKUP

后处理

  1. temperatureThe resulting suspension was heated
  2. temperatureat refluxing temperature
  3. customto react for 48 h
  4. customthe reaction mixture was partitioned between ethyl acetate and water
  5. washThe organic phase was washed repeatedly with water
  6. dry with materialdried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated by rotary evaporation