HRID840974

反应详情

EQUATION

反应方程式

HRID 840974 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Ethyl diethylphosphonoacetate (1.67 g, 7.42 mmol) was added dropwise to a solution of potassium tert-butoxide (0.83 g, 7.42 mmol) in tetrahydrofuran (10 ml), followed by stirring at room temperature for 10 minutes. Then, a solution of benzylacetone (1.00 g, 6.75 mmol) in tetrahydrofuran (10 ml) was added drop-wise thereto, and the resulting mixture was stirred at room temperature for 1 hour and then heated under reflux for another 1 hour. The reaction mixture was poured into a 5% aqueous potassium hydrogensulfate solution and extracted with ethyl acetate. The extract solution was washed with water and an aqueous sodium chloride solution and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 1.82 g of ethyl 5-phenyl-3-methyl-2-pentenoate.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred at room temperature for 1 hour
  2. temperatureheated
  3. temperatureunder reflux for another 1 hour
  4. extractionextracted with ethyl acetate
  5. washThe extract solution was washed with water
  6. dry with materialan aqueous sodium chloride solution and dried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off under reduced pressure