Hydrazine hydrate (1:1) → HCID 178430911, compound

HRID 498968Notes

Reaction equation

HRID 498968 reaction equation
C(O[CH:4]=[C:5]([CH3:12])[C:6](=O)[C:7]([F:10])([F:9])[F:8])C.O.[NH2:14][NH2:15]>C(O)C>[CH3:12][C:5]1[C:6]([C:7]([F:10])([F:9])[F:8])=[N:14][NH:15][CH:4]=1

Participants

4

Reactant 2

HCID 24654Hydrazine hydrate (1:1)HCID 713464954-Ethoxy-1,1,1-trifluoro-3-methylbut-3-EN-2-one

Product 1

HCID 178430911HCID 178430911, compoundYield 86.7%

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

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%).

Workup

  1. distillationThe ethanol was distilled off under reduced pressure
  2. customthe residue was separated with ethyl acetate and water
  3. washThe organic layer was washed with water twice
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationThe solvent was distilled off under reduced pressure

Sources & evidence

ORD record
ord-f73a2f82c4904d77922fabd1920c4a52
Source dataset
uspto-grants-2010_08
Patent number
US07767626B2

Reaction notes

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