反应详情

A mixture of 1-(2-methoxyphenyl)piperazine hydrochloride (9.10 g, 39.78 mmol), ethyl 3-bromopropionate (7.29 g, 5.14 mL, 40.29 mmol), potassium carbonate (20.00 g, 144.70 mmol) and a catalytic amount of potassium iodide in acetonitrile (80 mL) was heated at reflux for 18 hrs. After cooling at room temperature the solvent was evaporated under reduced pressure and the residue was taken up in dichloromethane. The organic phase was washed with water, dried over MgSO4 and evaporated to dryness. The resulting orange oil was purified by flash chromatography (Silica gel 60 Å, 45 μm, 50% ethyl acetate in hexane) and afforded 8.30 g (71%) ethyl 3-[4-(2-methoxyphenyl)piperazino]propanoate D1 as an oil.

1. temperatureat reflux for 18 hrs
2. customwas evaporated under reduced pressure
3. washThe organic phase was washed with water
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customThe resulting orange oil was purified by flash chromatography (Silica gel 60 Å, 45 μm, 50% ethyl acetate in hexane)