HRID365115
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureby cooling to room temperature
- extractionwas extracted with toluene (50 ml)
- extractionThe toluene extract
- washwas washed with water
- dry with materialdried over anhydrous sodium sulfate
- extractionThe toluene extract
- concentrationwas concentrated under reduced pressure
- customto give an oily residue
- customThe residue was purified by silica gel column chromatography