HRID1156857

反应详情

EQUATION

反应方程式

HRID 1156857 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

In a mixture of 3 g of 5-methylanthranilic acid in 30 ml of chloroform is dissolved 3 ml of triethylamine, to this mixture is added a solution of 4.2 g of 3,4-dimethoxycinnamoylchloride in chloroform under cooling. The mixture is stirred at room temperature for 2 hours and then heated under reflux for 2 hours. The reaction mixture is concentrated under a reduced pressure, to the residue is added water and hydrochloric acid is added to make the mixture the weakly acidic. The precipitated crystals are collected by filtration recrystallized from ethanol to obtain 4.8 g of N-(3,4-dimethoxycinnamoyl)-5-methylanthranilic acid as pale yellow needles.

WORKUP

后处理

  1. temperatureunder cooling
  2. temperatureheated
  3. temperatureunder reflux for 2 hours
  4. concentrationThe reaction mixture is concentrated under a reduced pressure, to the residue
  5. additionis added water and hydrochloric acid
  6. additionis added
  7. filtrationThe precipitated crystals are collected by filtration
  8. customrecrystallized from ethanol