Реакция #792153

ord-b43775164adb4ab08be9ccdf83415156

Уравнение реакции

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
Выход 62.2%
FC(F)(F)c1ccn(-c2ncccc2C(F)(F)F)n1
3-Trifluoromethyl-2-[3-(trifluoromethyl)-1H-pyrazol-1-yl]pyridine
Выход 62.2%

Растворители

Условия реакции

Температура
100°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ДругоеThe cooled reaction mixture
  2. 2
    ЭкстракцияThe mixture was extracted twice with ether (100 mL)
  3. 3
    Промывкаthe combined ether extracts were washed twice with water (100 mL)
  4. 4
    СушкаThe organic layer was dried with magnesium sulfate
  5. 5
    Концентрированиеconcentrated to an oil

Методика

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.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US09173400B2uspto-grants-2015_11