HRID27464

反应详情

EQUATION

反应方程式

HRID 27464 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

10.5 g of 4-(2-aminoethyl)-benzoic acid methyl ester-hydrochloride were suspended in 40 ml of dioxane and 20 ml of acetone and the suspension was combined with 8 ml of pyridine. To this suspension, a solution of 10 g of 2-ethoxy-5-chloro-benzoyl chloride in a small amount of acetone was added dropwise, while stirring, and the whole was heated for 2 hours under reflux. After cooling, the mixture was concentrated under reduced pressure, combined with ice-water, filtered with suction, stirred with dilute hydrochloric acid and with a NaHCO3 solution and the resulting product was again filtered off with suction and recrystallized from ethanol. The 4-(2-<2-ethoxy-5-chloro-benzamido>-ethyl)-benzoic acid methyl ester obtained was found to melt at 110° C.

WORKUP

后处理

  1. temperaturethe whole was heated for 2 hours
  2. temperatureunder reflux
  3. temperatureAfter cooling
  4. concentrationthe mixture was concentrated under reduced pressure
  5. filtrationfiltered with suction
  6. stirringstirred with dilute hydrochloric acid and with a NaHCO3 solution
  7. filtrationthe resulting product was again filtered off with suction
  8. customrecrystallized from ethanol