HRID5429
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 suspension of cysteamine hydrochloride (2.95 g, 26 mmoles) in ethanol (100 ml) was added 60% sodium hydride (oily; 2.08 g, 26 mmoles) with stirring under ice-cooling and the mixture was stirred for 5 minutes. 5-chloro-2-methylimidazo[1,2-a]pyridine (3.33 g, 20 mmoles) was added to the mixture, followed by heating at reflux for 3 hours. After the solvent was distilled off, chloroform was added to the residue which was washed with 1N-NaOH and dried over anhydrous potassium carbonate. After the solvent was distilled off, the residue was purified by column chromatography (eluent: ethyl acetate/ethanol/triethylamine=6:2:1) to obtain 2.2 g of the desired product (53.6%, brown oily product).
WORKUP
后处理
- temperaturecooling
- stirringthe mixture was stirred for 5 minutes
- temperatureby heating
- temperatureat reflux for 3 hours
- distillationAfter the solvent was distilled off
- additionchloroform was added to the residue which
- washwas washed with 1N-NaOH
- dry with materialdried over anhydrous potassium carbonate
- distillationAfter the solvent was distilled off
- customthe residue was purified by column chromatography (eluent: ethyl acetate/ethanol/triethylamine=6:2:1)