反应详情

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.

1. temperaturewas refluxed under nitrogen for 18 hours
2. temperatureThe mixture was then cooled
3. filtrationfiltered
4. customthe solvent removed in vacuo
5. dissolutionThe residue was dissolved in CH2Cl2 (200 ml)
6. washwashed with water (50 ml)
7. customDrying
8. customremoval of the solvent