反应详情

3 g (15.7 mmol) of 5-bromo-thiophene-2-carbaldehyde were dissolved in 30 ml of pyridine and 1.96 g (18.8 mmol) of malonic acid and 133 mg (1.6 mmol) of piperidine was added. The reaction mixture was boiled under reflux for 6 h. After cooling to room temperature, it was poured into a mixture of ice and concentrated aqueous hydrochloric acid whereupon the product precipitated. The product was isolated by filtration, dissolved in ethyl acetate, and the solution was washed with 0.1 M hydrochloric acid. The organic phase was dried with sodium sulfate, filtered and the solvent was removed under reduced pressure. Yield: 3.0 g.

1. temperatureunder reflux for 6 h
2. customprecipitated
3. customThe product was isolated by filtration
4. washthe solution was washed with 0.1 M hydrochloric acid
5. dry with materialThe organic phase was dried with sodium sulfate
6. filtrationfiltered
7. customthe solvent was removed under reduced pressure