反应 #657307

ord-1d076a840bc2483f9538a4bf5b21a9e0

反应方程式

COC(=O)CC(=O)c1ccc(F)cc1
methyl 3-(4-fluorophenyl)-3-oxopropanoate
NN.O
hydrazine hydrate
CCOCC
diethyl ether
Oc1cc(-c2ccc(F)cc2)n[nH]1
3-(4-fluorophenyl)-1H-pyrazol-5-ol

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度is heated 3 h
  2. 2
    温度under reflux
  3. 3
    温度The resulting suspension is cooled down
  4. 4
    过滤The precipitate is filtered off
  5. 5
    干燥dried in vacuo and 9 g (100%) of 3-(4-fluorophenyl)-1H-pyrazol-5-ol
  6. 6
    其他are obtained as white solid

实验过程

A mixture of methyl 3-(4-fluorophenyl)-3-oxopropanoate (10.0 g, 0.051 mol) and hydrazine hydrate (1.1 eq, 2.8 g, 0.056 mol) in 20 mL glacial acetic acid is heated 3 h under reflux. The resulting suspension is cooled down and 10 mL diethyl ether is added. The precipitate is filtered off, dried in vacuo and 9 g (100%) of 3-(4-fluorophenyl)-1H-pyrazol-5-ol are obtained as white solid.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09023844B2uspto-grants-2015_05