反应 #44697

ord-63c7feb226134404a5bf0269df3955a5

反应方程式

N#Cc1c(F)cccc1F
2,6-difluorobenzonitrile
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Nc1ccc(O)c(Cl)c1
3-chloro-4-hydroxyaniline
N#Cc1c(F)cccc1Oc1ccc(N)cc1Cl
2-(4-Amino-2-chlorophenoxy)-6-fluorobenzonitrile

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度the mixture is heated
  2. 2
    温度at reflux for 45 min
  3. 3
    过滤The mixture is filtered
  4. 4
    洗涤the filtercake is washed with ethyl acetate and DCM
  5. 5
    其他The solvent is removed under reduced pressure

实验过程

1.00 g (7.19 mmol) of 2,6-difluorobenzonitrile is initially charged in 10 ml of acetonitrile. 1.99 g (14.4 mmol) of potassium carbonate and 1.03 g (7.19 mmol) of 3-chloro-4-hydroxyaniline are added, and the mixture is heated at reflux for 45 min. The mixture is filtered and the filtercake is washed with ethyl acetate and DCM. The solvent is removed under reduced pressure and the residue is by column chromatography (silica gel 60, gradient column: mobile phase: DCM:petroleum ether=2:1, then DCM).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07737153B2uspto-grants-2010_06