HRID244809

反应详情

EQUATION

反应方程式

HRID 244809 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

7-Bromo-N4-(3-isopropoxypropyl)quinoline-3,4-diamine (45 g) was dissolved in acetonitrile (1.3 L) and triethylamine (19.4 mL). Ethoxyacetyl chloride (18.0 g) was added dropwise to the solution and the reaction was stirred for 16 hours. The solvent was removed under reduced pressure to afford a tan solid. The solid was added to a solution of ethanol (1 L) and triethylamine (77.5 mL) and heated at reflux for 4 hours. The solvent was removed under reduced pressure. Water was added to the solid residue and the crude product was recovered by filtration. Recrystallization from acetonitrile yielded 36.25 g of 7-bromo-2-ethoxymethyl-1-(3-isopropoxypropyl)-1H-imidazo[4,5-c]quinoline as a tan crystalline solid.

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. customto afford a tan solid
  3. temperatureheated
  4. temperatureat reflux for 4 hours
  5. customThe solvent was removed under reduced pressure
  6. additionWater was added to the solid residue
  7. filtrationthe crude product was recovered by filtration
  8. customRecrystallization from acetonitrile