HRID1006048

反应详情

EQUATION

反应方程式

HRID 1006048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a mixture of 2-benzyloxy-5-bromophenylacetic acid (3.2 g) in toluene (100 ml) was added thionyl chloride (1.0 ml) and DMF (3 drops). The reaction was stirred at 80° C. for 1 hour and cooled to ambient temperature ethyl 4-aminobenzoate (2.0 g) and triethylamine (2 ml) were added to the reaction mixture with stirring. After standing for 18 hours, the mixture was diluted with dichloromethane and washed with water, 1N HCl solution, water and sautrated aqueous NaHCO3 solution. The organic extract was dried (MgSO4), filtered and evaporated and the residue purified by trituration with diethyl ether to give ethyl 4-[2-benzyloxy-5-bromophenylacetamido]benzoate (2.0 g) mpt. 174-176° C.

WORKUP

后处理

  1. additionwere added to the reaction mixture
  2. stirringwith stirring
  3. waitAfter standing for 18 hours
  4. washwashed with water, 1N HCl solution, water
  5. extractionThe organic extract
  6. dry with materialwas dried (MgSO4)
  7. filtrationfiltered
  8. customevaporated
  9. customthe residue purified by trituration with diethyl ether