反応 #792153

ord-b43775164adb4ab08be9ccdf83415156

反応方程式

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

反応条件

温度
100°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The cooled reaction mixture
  2. 2
    抽出The mixture was extracted twice with ether (100 mL)
  3. 3
    洗浄the combined ether extracts were washed twice with water (100 mL)
  4. 4
    乾燥The organic layer was dried with magnesium sulfate
  5. 5
    濃縮concentrated to an oil

実験手順

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.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09173400B2uspto-grants-2015_11