HRID497058

反应详情

EQUATION

反应方程式

HRID 497058 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Potassium carbonate and benzyl bromoacetate were added to DMF solution of ethyl (4-aminophenoxy)acetate and stirred under heating. After adding water and ethyl acetate to the reaction mixture, the organic layer was separated, washed and dried, and then the solvent was evaporated under a reduced pressure. Dichloromethane solution of the thus obtained crude product was mixed with TEA, 4-fluorobenzoyl chloride was added dropwise thereto under ice-cooling and then the reaction solution was stirred. After adding 1 M hydrochloric acid to the reaction solution, the organic layer was separated, washed and dried, and then the solvent was evaporated under a reduced pressure. By purifying the thus obtained crude product by SCG, ethyl {4-[benzyloxycarbonylmethyl-(4-fluorobenzoyl)amino]phenoxy}acetate (colorless oil) was obtained.

WORKUP

后处理

  1. temperatureunder heating
  2. customthe organic layer was separated
  3. washwashed
  4. customdried
  5. customthe solvent was evaporated under a reduced pressure
  6. customDichloromethane solution of the thus obtained crude product
  7. additionwas added dropwise
  8. temperatureunder ice-cooling
  9. stirringthe reaction solution was stirred
  10. customthe organic layer was separated
  11. washwashed
  12. customdried
  13. customthe solvent was evaporated under a reduced pressure
  14. customBy purifying the
  15. customthus obtained crude product by SCG