反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- additionwas added
- distillationwas distilled off under reduced pressure and chloroform
- additionwas added to the residue
- washAfter thoroughly washing the chloroform solution with water, it
- dry with materialwas dried with anhydrous magnesium sulfate
- distillationChloroform was distilled off under reduced pressure
- customthe residue was purified by silica gel column chromatography
- customfollowed by recrystallization from a mixed solvent of ethanol and ether