HRID2166824

反应详情

EQUATION

反应方程式

HRID 2166824 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2.85 g (16.5 millimoles) of quinoline-2-carboxylic acid are dissolved in 200 ml of absolute tetrahydrofuran, 2.7 g (16.5 millimoles) of N,N'-carbonyl-diimidazole are added and the mixture is stirred for 45 minutes at room temperature. A solution of 3.75 g (16.5 millimoles) of 2-(2',6'-dichlorophenylamino)-2-imidazoline in 75 ml of absolute tetrahydrofuran is then added dropwise and the batch is stirred overnight. Thereafter, the reaction solution is freed from solvent on a rotary evaporator and the oily residue is introduced into 200 ml of an 0.5% strength sodium bicarbonate solution. The crystalline crude product (5.2 g) is filtered off and recrystallized from N,N-dimethylacetamide/isopropanol, and the crystals are washed with cold isopropanol. 3.3 g of 1-(quinolin-2-oyl)-2-(2',6'-dichlorophenylamino)-2-imidazoline are obtained, melting point 197°-198° C.

WORKUP

后处理

  1. stirringthe batch is stirred overnight
  2. customThereafter, the reaction solution is freed from solvent on a rotary evaporator
  3. additionthe oily residue is introduced into 200 ml of an 0.5% strength sodium bicarbonate solution
  4. filtrationThe crystalline crude product (5.2 g) is filtered off
  5. customrecrystallized from N,N-dimethylacetamide/isopropanol
  6. washthe crystals are washed with cold isopropanol