HRID1196642

反应详情

EQUATION

反应方程式

HRID 1196642 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

3.6 g of powdered potassium carbonate, 1.5 g of finely powdered potassium iodide and 27 g of methyl 2-chloroethylcarbamate are added to a solution of 2.6 g of 4-(4-fluorophenoxy)phenol in 120 ml of dimethyl formamide, and the reaction mixture is heated for 15 hours to 95° C. The cooled reaction mixture is poured into ice-water and extracted repeatedly with ether. The combined ether phases are washed with water, dried over sodium sulfate, and the solvent is completely removed by distillation. After filtration over silica gel, the crude product is recrystallised from diethyl ether/hexane to give methyl 2-[4-(4-fluorophenoxy)phenoxy]-1-ethylcarbamate with a melting point of 64°-66° C.

WORKUP

后处理

  1. temperaturethe reaction mixture is heated for 15 hours to 95° C
  2. customThe cooled reaction mixture
  3. extractionextracted repeatedly with ether
  4. washThe combined ether phases are washed with water
  5. dry with materialdried over sodium sulfate
  6. customthe solvent is completely removed by distillation
  7. filtrationAfter filtration over silica gel
  8. customthe crude product is recrystallised from diethyl ether/hexane