反应 #586150

ord-f73a2f82c4904d77922fabd1920c4a52

反应方程式

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
收率 86.7%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    workup.DISTILLATIONThe ethanol was distilled off under reduced pressure
  2. 2
    其他the residue was separated with ethyl acetate and water
  3. 3
    洗涤The organic layer was washed with water twice
  4. 4
    干燥dried over anhydrous magnesium sulfate
  5. 5
    workup.DISTILLATIONThe solvent was distilled off under reduced pressure

实验过程

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%).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07767626B2uspto-grants-2010_08