HRID1156858

反应详情

EQUATION

反应方程式

HRID 1156858 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 3.4 g of 4-chloroanthranilic acid in 50 ml of tetrahydrofuran is dissolved 3 ml of triethylamine, to this mixture is added slowly a solution of 4.5 g of 3,4-dimethoxycinnamoylchloride in tetrahydrofuran under room temperature, and this solution is stirred at room temperature for 5 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 and recrystallized from a mixture of dimethylformamide and water to obtain 5.9 g of N-(3,4-dimethoxycinnamoyl)-4-chloroanthranilic acid as colorless prisms.

WORKUP

后处理

  1. concentrationThe reaction mixture is concentrated under a reduced pressure, to the residue
  2. additionis added water and hydrochloric acid
  3. additionis added
  4. filtrationThe precipitated crystals are collected by filtration
  5. customrecrystallized from a mixture of dimethylformamide and water