反应 #67958

反应方程式

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

溶剂

water

ethyl acetate

反应条件

后处理

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
   其他The organic layer was separated
8. 8
   洗涤washed with an aqueous saturated sodium chloride solution
9. 9
   干燥dried over anhydrous magnesium sulfate
10. 10
    其他the solvent was removed under reduced pressure
11. 11
    其他The residue thus obtained
12. 12
    其他was purified by silica gel column chromatography [eluent; chloroform:methanol=50:1]

实验过程

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.

来源