Potassium Carbonate → HCID 22250324, compound
Reaction equation
Cl[C:2]1[C:7]([C:8]([F:11])([F:10])[F:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[F:12][C:13]([F:20])([F:19])[C:14]1[CH:18]=[CH:17][NH:16][N:15]=1.C(=O)([O-])[O-].[K+].[K+]>>[F:9][C:8]([F:11])([F:10])[C:7]1[C:2]([N:16]2[CH:17]=[CH:18][C:14]([C:13]([F:20])([F:19])[F:12])=[N:15]2)=[N:3][CH:4]=[CH:5][CH:6]=1Participants
4
Conditions
- Temperature
- 100 °C
Procedure
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 as oil.
Workup
- customThe cooled reaction mixture
- extractionThe mixture was extracted twice with ether (100 mL)
- washthe combined ether extracts were washed twice with water (100 mL)
- dry with materialThe organic layer was dried with magnesium sulfate
- concentrationconcentrated to an oil
Sources & evidence
- ORD record
- ord-74db66cfc1aa4398bc4031cc4b1f1409
- Source dataset
- uspto-grants-2014_01
- Patent number
- US08637552B2
Reaction notes
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