반응 #67958

반응 방정식

N,N-dimethylformamide

2-(2-bromoethylthio)thiophene

potassium carbonate

1-(trifluoroacetyl)piperidine-4-amine hydrochloride

potassium carbonate

→

N-(2-(2-thienylthio)ethyl)-1-(trifluoroacetyl)piperidine-4-amine

용매

water

ethyl acetate

반응 조건

후처리

1. 1
   workup.ADDITIONwere added
2. 2
   온도under cooling with ice
3. 3
   온도under cooling with ice
4. 4
   workup.STIRRINGthe mixture was stirred for 45 minutes
5. 5
   workup.STIRRINGstirred at 70° C. for 3 hours
6. 6
   온도The reaction mixture was cooled to room temperature
7. 7
   기타The organic layer was separated
8. 8
   세척washed with an aqueous saturated sodium chloride solution
9. 9
   건조dried over anhydrous magnesium sulfate
10. 10
    기타the solvent was removed under reduced pressure
11. 11
    기타The residue thus obtained
12. 12
    기타was purified by silica gel column chromatography [eluent; chloroform:methanol=50:1]

실험 절차

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.

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