反应详情

To a solution of ethyl 4,6-dichloronicotinate (S13, 1.0 g) synthesized according to the method described in US200549419 A1 and N,N-diisopropylethylamine (2.37 mL) in acetonitrile (10 mL), propylamine (0.90 mL) was added under ice cooling, and the mixture was stirred at the same temperature for 30 minutes, and then stirred at room temperature for 5 hours and 30 minutes. To the reaction mixture, water and ethyl acetate were added. The organic layer was separated, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (eluent, 90% hexane/10% ethyl acetate) to obtain ethyl 6-chloro-4-(propylamino)nicotinate (S14, 1.1 g).

1. additionwas added under ice cooling
2. stirringstirred at room temperature for 5 hours and 30 minutes
3. customThe organic layer was separated
4. dry with materialdried over anhydrous sodium sulfate
5. customthe solvent was evaporated under reduced pressure
6. customThe obtained residue was purified by silica gel column chromatography (eluent, 90% hexane/10% ethyl acetate)