반응 #1005944

ord-2833baeb11584e4787c4da4f052e18c2

반응 방정식

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
수율 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
수율 42.5%

반응 조건

온도
110°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도After cooling the mixture to room temperature
  2. 2
    세척washed with water three times
  3. 3
    건조The organic layer was dried over anhydrous magnesium sulfate
  4. 4
    기타The solvent was evaporated off under reduced pressure
  5. 5
    기타the residue was then purified by a column chromatography

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US09271499B2uspto-grants-2016_03