反应 #1005944

ord-2833baeb11584e4787c4da4f052e18c2

反应方程式

FC(F)(F)C1(c2cc(Cl)cc(Cl)c2)CCNC1
3-(3,5-Dichlorophenyl)-3-(trifluoromethyl)pyrrolidine
N#Cc1ccc(F)cc1C(F)(F)F
4-fluoro-2-trifluoromethylbenzonitrile
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CN(C)C=O
N,N-dimethylformamide
N#Cc1ccc(N2CCC(c3cc(Cl)cc(Cl)c3)(C(F)(F)F)C2)cc1C(F)(F)F
title compound
收率 42.5%
N#Cc1ccc(N2CCC(c3cc(Cl)cc(Cl)c3)(C(F)(F)F)C2)cc1C(F)(F)F
4-[3-(3,5-dichlorophenyl)-3-(trifluoromethyl)pyrrolidin-1-yl]-2-(trifluoromethyl)-benzonitrile
收率 42.5%

反应条件

温度
110°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度After cooling the mixture to room temperature
  2. 2
    洗涤washed with water three times
  3. 3
    干燥The organic layer was dried over anhydrous magnesium sulfate
  4. 4
    其他The solvent was evaporated off under reduced pressure
  5. 5
    其他the residue was then purified by a column chromatography

实验过程

3-(3,5-Dichlorophenyl)-3-(trifluoromethyl)pyrrolidine (5.6 g), 4-fluoro-2-trifluoromethylbenzonitrile (4.5 g) and potassium carbonate (5.4 g) were added to N,N-dimethylformamide (50 mL), and the mixture was stirred at 110° C. for 4 hours. After cooling the mixture to room temperature, the solution was diluted with ethyl acetate and washed with water three times. The organic layer was dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was then purified by a column chromatography to obtain the title compound (3.8 g).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09271499B2uspto-grants-2016_03