HRID365115

反应详情

EQUATION

反应方程式

HRID 365115 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

A mixture of 4-(3,5-difluorophenoxy)phenol (0.50 g), ethyl N-2-chloroethylcarbamate (0.375 g), potassium carbonate (0.621 g) and anhydrous dimethylformamide (10 ml) was stirred at 100° C. for 3 hours, followed by cooling to room temperature. Ice-water (50 ml) was poured to the resultant mixture, which was extracted with toluene (50 ml). The toluene extract was washed with water and dried over anhydrous sodium sulfate. The toluene extract was concentrated under reduced pressure to give an oily residue. The residue was purified by silica gel column chromatography to give 0.605 g of ethyl N-2-[4-(3,5-difluorophenoxy)phenoxy]ethylcarbamate as a colorless liquid. nD25.5 1.5305.

WORKUP

后处理

  1. temperatureby cooling to room temperature
  2. extractionwas extracted with toluene (50 ml)
  3. extractionThe toluene extract
  4. washwas washed with water
  5. dry with materialdried over anhydrous sodium sulfate
  6. extractionThe toluene extract
  7. concentrationwas concentrated under reduced pressure
  8. customto give an oily residue
  9. customThe residue was purified by silica gel column chromatography