反应 #543607
ord-c1c72bb6d7684682909cb1d87fe96f0c
反应方程式
piperazine
4-(2-bromo-ethoxy)-1,3-difluoro benzene
K2CO3
→
desired product
收率 73.0%
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温度was refluxed under nitrogen for 18 hours
- 2温度The mixture was then cooled
- 3过滤filtered
- 4其他the solvent removed in vacuo
- 5workup.DISSOLUTIONThe residue was dissolved in CH2Cl2 (200 ml)
- 6洗涤washed with water (50 ml)
- 7其他Drying
- 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.