反应 #543607

ord-c1c72bb6d7684682909cb1d87fe96f0c

反应方程式

C1CNCCN1
piperazine
Fc1ccc(OCCBr)c(F)c1
4-(2-bromo-ethoxy)-1,3-difluoro benzene
O=C([O-])[O-].[K+].[K+]
K2CO3
Fc1ccc(OCCN2CCNCC2)c(F)c1
desired product
收率 73.0%
Fc1ccc(OCCN2CCNCC2)c(F)c1
1-[2-(2,4-difluoro-phenoxy)-ethyl]-piperazine
收率 73.0%

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度was refluxed under nitrogen for 18 hours
  2. 2
    温度The mixture was then cooled
  3. 3
    过滤filtered
  4. 4
    其他the solvent removed in vacuo
  5. 5
    workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (200 ml)
  6. 6
    洗涤washed with water (50 ml)
  7. 7
    其他Drying
  8. 8
    其他removal of the solvent

实验过程

A mixture of piperazine (8.7 g, 101.26 mmol) in butanone (70 ml), 4-(2-bromo-ethoxy)-1,3-difluoro benzene (6.0 g, 25.31 mmol), anhydrous K2CO3 (3.5 g, 25.31 mmol) and KI (4.2 g, 25.31 mmol) was refluxed under nitrogen for 18 hours. The mixture was then cooled and filtered and the solvent removed in vacuo. The residue was dissolved in CH2Cl2 (200 ml) and washed with water (50 ml). Drying and removal of the solvent followed by chromatography (CH2Cl2:CH3OH:NH4OH 10:1) afforded desired product in 73% yield.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07186726B2uspto-grants-2007_03