反应详情

To 2 mL of an N,N-dimethylformamide solution containing 0.14 g of 2-(2-bromoethylthio)thiophene, 95 mg of potassium carbonate and 0.16 g of 1-(trifluoroacetyl)piperidine-4-amine hydrochloride were added under cooling with ice, and the mixture was stirred at room temperature for 40 minutes. Thereto was added 95 mg of potassium carbonate under cooling with ice, and the mixture was stirred for 45 minutes, and stirred at 70° C. for 3 hours. The reaction mixture was cooled to room temperature, and then ethyl acetate and water were added thereto. The organic layer was separated, washed with an aqueous saturated sodium chloride solution, and dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The residue thus obtained was purified by silica gel column chromatography [eluent; chloroform:methanol=50:1] to obtain 62 mg of a yellow oily substance, N-(2-(2-thienylthio)ethyl)-1-(trifluoroacetyl)piperidine-4-amine.

1. additionwere added
2. temperatureunder cooling with ice
3. temperatureunder cooling with ice
4. stirringthe mixture was stirred for 45 minutes
5. stirringstirred at 70° C. for 3 hours
6. temperatureThe reaction mixture was cooled to room temperature
7. customThe organic layer was separated
8. washwashed with an aqueous saturated sodium chloride solution
9. dry with materialdried over anhydrous magnesium sulfate
10. customthe solvent was removed under reduced pressure
11. customThe residue thus obtained
12. customwas purified by silica gel column chromatography [eluent; chloroform:methanol=50:1]