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
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
- temperatureunder heating
- customthe organic layer was separated
- washwashed
- customdried
- customthe solvent was evaporated under a reduced pressure
- customDichloromethane solution of the thus obtained crude product
- additionwas added dropwise
- temperatureunder ice-cooling
- stirringthe reaction solution was stirred
- customthe organic layer was separated
- washwashed
- customdried
- customthe solvent was evaporated under a reduced pressure
- customBy purifying the
- customthus obtained crude product by SCG