HRID1156854

反应详情

EQUATION

反应方程式

HRID 1156854 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1.3 g of methyl 5-chloroanthranilate and 1.8 g of 3,4,5-trimethoxybenzoylchloride in 30 ml of tetrahydrofuran is added 1.5 g of triethylamine under cooling, and the mixture is stirred at room temperature for 2 hours and then heated under reflux for 1 hour. The reaction mixture is concentrated under reduced pressure and to the residue is added water. The precipitated crystals are collected by filtration and recrystallized from a mixture of chloroform and ether to obtain 1.4 g of methyl N-(3,4,5-trimethoxybenzoyl)-5-chloroanthranilate as colorless prisms.

WORKUP

后处理

  1. temperatureunder cooling
  2. temperatureheated
  3. temperatureunder reflux for 1 hour
  4. concentrationThe reaction mixture is concentrated under reduced pressure and to the residue
  5. additionis added water
  6. filtrationThe precipitated crystals are collected by filtration
  7. customrecrystallized from a mixture of chloroform and ether