Reaktion #792153

ord-b43775164adb4ab08be9ccdf83415156

Reaktionsgleichung

FC(F)(F)c1cccnc1Cl
2-chloro-3-trifluoromethylpyridine
FC(F)(F)c1cc[nH]n1
3-trifluoromethylpyrazole
O=C([O-])[O-].[K+].[K+]
potassium carbonate
FC(F)(F)c1ccn(-c2ncccc2C(F)(F)F)n1
title compound
Ausbeute 62.2%
FC(F)(F)c1ccn(-c2ncccc2C(F)(F)F)n1
3-Trifluoromethyl-2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine
Ausbeute 62.2%

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe cooled reaction mixture
  2. 2
    ExtraktionThe mixture was extracted twice with ether (100 mL)
  3. 3
    Waschenthe combined ether extracts were washed twice with water (100 mL)
  4. 4
    TrocknenThe organic layer was dried with magnesium sulfate
  5. 5
    Einengenconcentrated to an oil

Vorschrift

A mixture of 2-chloro-3-trifluoromethylpyridine (3.62 g., 21 mmol), 3-trifluoromethylpyrazole (2.7 g., 20 mmol), and potassium carbonate (6.0 g, 43 mmol) were heated at 100° C. for 18 h. The cooled reaction mixture was added to ice/water (100 mL). The mixture was extracted twice with ether (100 mL) and the combined ether extracts were washed twice with water (100 mL). The organic layer was dried with magnesium sulfate and concentrated to an oil. Chromatography on silica gel with hexanes:ethyl acetate 8:1 to 4:1 as eluent gave the title compound (3.5 g) as an oil.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09173400B2uspto-grants-2015_11