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 solution of 1.25 g (4.32 mmol) of 3-[4-(imidazo[1,2-a]pyridin-8-yloxy)butyl]thiazolidine-2,4-dione and 0.39 ml (4.32 mmol) of 1-butanal in 20 ml of ethanol, 0.036 ml (0.43 mmol) of pyrrolidine was added at 60° C., followed by refluxing for 19 hours (1 and 2 hours later, 0.39 ml (4.32 mmol) was further added; 3 hours later, 0.39 ml (4.32 mmol) of 1-butanal and 0.036 ml (0.43 mmol) of pyrrolidine were further added). After the reaction mixture was cooled, the solvent was distilled off. The residue was dissolved in dichloromethane, washed with purified water and dried, after which the solvent was distilled off. The residue was purified by column chromatography (eluent, n-hexane/ethyl acetate=1/4), after which the solvent was distilled off, to yield 0.17 g (11.5%, yellow oily substance) of the desired product.
WORKUP
后处理
- temperatureby refluxing for 19 hours (1 and 2 hours later
- addition0.39 ml (4.32 mmol) was further added
- temperatureAfter the reaction mixture was cooled
- distillationthe solvent was distilled off
- dissolutionThe residue was dissolved in dichloromethane
- washwashed with purified water
- customdried
- distillationafter which the solvent was distilled off
- customThe residue was purified by column chromatography (eluent, n-hexane/ethyl acetate=1/4)
- distillationafter which the solvent was distilled off