反応 #1005944

ord-2833baeb11584e4787c4da4f052e18c2

反応方程式

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
収率 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
収率 42.5%

反応条件

温度
110°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

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).

出典

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