反应详情

4.28 mg of ethyl 5-chloro-3-oxopentanoate was dissolved in 40 ml of ethanol, 2.94 g of 2-amino-5-bromopyridine was added and the mixture was stirred all night by heating under reflux. The mixture was cooled down to room temperature, and the solvents were distilled outunder reduced pressure. Ethyl acetate followed by saturated sodium bicarbonate aqueous solution were added. Organic layer was dried with anhydrous sodium sulfate, and the solvents were distilled outunder reduced pressure. The obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=50:50) to obtain 990 mg of the above compound as crude product.

1. temperatureby heating
2. temperatureunder reflux
3. distillationthe solvents were distilled outunder reduced pressure
4. additionwere added
5. dry with materialOrganic layer was dried with anhydrous sodium sulfate
6. distillationthe solvents were distilled outunder reduced pressure
7. customThe obtained residues were purified by preparative thin-layer silicagel chromatography (hexane:ethyl acetate=50:50)