HRID1797338

反应详情

EQUATION

反应方程式

HRID 1797338 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

26.8 g (75.52 mmol) methyl (2E)-3-{4-[(8-chloroctyl)oxy]-3-methoxyphenyl}-2-propenoate was dissolved in 1000 ml acetone. 65.16 g (435.15 mmol) sodium iodide were added. The reaction suspension was heated at reflux temperature for 24 hours. The reaction mixture was partitioned between diethylether and water. The organic phase was washed repeatedly with water, dried over sodium sulfate, filtered and concentrated by rotary evaporation. The crude product was recrystallised from 2-propanol yielded 30.1 g (90%) methyl (2E)-3-{4-[(8-iodoctyl)oxy]-3-methoxyphenyl}-2-propenoate as white crystals.

WORKUP

后处理

  1. temperatureThe reaction suspension was heated
  2. temperatureat reflux temperature for 24 hours
  3. customThe reaction mixture was partitioned between diethylether and water
  4. washThe organic phase was washed repeatedly with water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated by rotary evaporation
  8. customThe crude product was recrystallised from 2-propanol