HRID542715

反应详情

EQUATION

反应方程式

HRID 542715 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 2.66 g of 6-acetamido-8-bromo-1,7-naphthyridine and 6.51 g of 1-piperazine ethanol, 180 ml of ethoxyethanol was added. The resultant mixture was refluxed with stirring for 45 minutes. After the reaction, ethoxyethanol was distilled off under reduced pressure and chloroform was added to the residue. After thoroughly washing the chloroform solution with water, it was dried with anhydrous magnesium sulfate. Chloroform was distilled off under reduced pressure and the residue was purified by silica gel column chromatography, followed by recrystallization from a mixed solvent of ethanol and ether to obtain 2.6 g of 6-acetamido-8-[4-(2-hydroxyethyl)-1-piperazinyl]-1,7-naphthyridine (Compound No. 22) as light yellowish crystals (yield: 82.5%).

WORKUP

后处理

  1. additionwas added
  2. distillationwas distilled off under reduced pressure and chloroform
  3. additionwas added to the residue
  4. washAfter thoroughly washing the chloroform solution with water, it
  5. dry with materialwas dried with anhydrous magnesium sulfate
  6. distillationChloroform was distilled off under reduced pressure
  7. customthe residue was purified by silica gel column chromatography
  8. customfollowed by recrystallization from a mixed solvent of ethanol and ether