تفاعل #67958

معادلة التفاعل

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

المذيبات

water

ethyl acetate

ظروف التفاعل

المعالجة

1. 1
   workup.ADDITIONwere added
2. 2
   درجة الحرارةunder cooling with ice
3. 3
   درجة الحرارةunder 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
   درجة الحرارةThe reaction mixture was cooled to room temperature
7. 7
   أخرىThe organic layer was separated
8. 8
   غسيلwashed with an aqueous saturated sodium chloride solution
9. 9
   تجفيفdried over anhydrous magnesium sulfate
10. 10
    أخرىthe solvent was removed under reduced pressure
11. 11
    أخرىThe residue thus obtained
12. 12
    أخرىwas purified by silica gel column chromatography [eluent; chloroform:methanol=50:1]

الإجراء التجريبي

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.

المصدر