Reaction #586150

ord-f73a2f82c4904d77922fabd1920c4a52

Solvents

Conditions

Detailed conditions
See reaction.notes.procedure_details.

Workup

  1. 1
    workup.DISTILLATIONThe ethanol was distilled off under reduced pressure
  2. 2
    Otherthe residue was separated with ethyl acetate and water
  3. 3
    WashThe organic layer was washed with water twice
  4. 4
    Dryingdried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

Procedure

1.7 g (10.2 mmol) of 4-ethoxy-3-methyl-1,1,1-trifluoro-3-buten-2-on and 0.6 g (12.0 mmol) hydrazine hydrate were stirred in 50 ml of ethanol at room temperature for 2 hours. The ethanol was distilled off under reduced pressure, and the residue was separated with ethyl acetate and water. The organic layer was washed with water twice and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 1.3 g of 4-methyl-3-trifluoromethylpyrazol (yield 86.7%).

Source

DOI: 10.6084/m9.figshare.5104873.v1Patent: US07767626B2uspto-grants-2010_08