反応 #67958

反応方程式

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

溶媒

water

ethyl acetate

反応条件

後処理

1. 1
   workup.ADDITIONwere added
2. 2
   温度under cooling with ice
3. 3
   温度under 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
   温度The reaction mixture was cooled to room temperature
7. 7
   その他The organic layer was separated
8. 8
   洗浄washed with an aqueous saturated sodium chloride solution
9. 9
   乾燥dried over anhydrous magnesium sulfate
10. 10
    その他the solvent was removed under reduced pressure
11. 11
    その他The residue thus obtained
12. 12
    その他was purified by silica gel column chromatography [eluent; chloroform:methanol=50:1]

実験手順

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.

出典