反应 #792153

ord-b43775164adb4ab08be9ccdf83415156

反应方程式

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

反应条件

温度
100°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The cooled reaction mixture
  2. 2
    萃取The mixture was extracted twice with ether (100 mL)
  3. 3
    洗涤the combined ether extracts were washed twice with water (100 mL)
  4. 4
    干燥The organic layer was dried with magnesium sulfate
  5. 5
    浓缩concentrated to an oil

实验过程

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.

来源

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