Реакция #586150

ord-f73a2f82c4904d77922fabd1920c4a52

Уравнение реакции

CCOC=C(C)C(=O)C(F)(F)F
4-ethoxy-3-methyl-1,1,1-trifluoro-3-buten-2-on
NN.O
hydrazine hydrate
Cc1c[nH]nc1C(F)(F)F
4-methyl-3-trifluoromethylpyrazol
Выход 86.7%

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

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

Методика

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%).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US07767626B2uspto-grants-2010_08