Reaction #1909809
ord-2734c8112b27427c90422f28efd949de
Reaction equation
3-(2,6-difluorophenyl)pyrazole
chloroacetonitrile
potassium carbonate
→
1-cyanomethyl-3-(2,6-difluorophenyl)pyrazole
Yield 47.7%
Reagents
None
Solvents
Conditions
Detailed conditions
See reaction.notes.procedure_details.
Workup
- 1Temperatureunder reflux for 5 hours
- 2workup.DISTILLATIONAfter acetonitrile was distilled off under reduced pressure, ethyl acetate
- 3workup.ADDITIONwas added to the residue, which
- 4Washwas then washed with a small amount of water
- 5DryingThe organic layer was dried over sodium sulfate
- 6workup.DISTILLATIONthe solvent was distilled off under reduced pressure
- 7OtherThe residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether
Procedure
3.0 g of 3-(2,6-difluorophenyl)pyrazole was dissolved in 20 ml of acetonitrile, and 2.52 g of chloroacetonitrile and 4.61 g of potassium carbonate were added thereto at room temperature, and heated under reflux for 5 hours. After acetonitrile was distilled off under reduced pressure, ethyl acetate was added to the residue, which was then washed with a small amount of water. The organic layer was dried over sodium sulfate, and the solvent was distilled off under reduced pressure. The residual product was recrystallized from a mixed solvent of isopropylether and diethyl ether to obtain 1.74 g of 1-cyanomethyl-3-(2,6-difluorophenyl)pyrazole.