反应详情

A mixture of 5.5 g (0.029 mol) of 1-(4-fluoro-3-methylphenyl)piperazine, 5.6 g (0.034 mol) of 5-(2-chloroethyl)-3-methyl-2-oxazolidinone, 12.1 g (0.114 mol) of anhydrous sodium carbonate, and 0.3 g (0.002 mol) of potassium iodide in 250 mL of 1-butanol was heated at reflux for 16 h. The mixture was concentrated under reduced pressure and the residue partitioned between 300 mL of benzene and 300 mL of water. The benzene layer was washed with water and brine, dried (MgSO4) and concentrated under reduced pressure to give a light-pink oil. The oil was converted to the oxalic acid salt and the solid was recrystallized from methanol to yield 10.0 g (81%) of white solid, mp 200°-203° C.

1. temperaturewas heated
2. temperatureat reflux for 16 h
3. concentrationThe mixture was concentrated under reduced pressure
4. customthe residue partitioned between 300 mL of benzene and 300 mL of water
5. washThe benzene layer was washed with water and brine
6. dry with materialdried (MgSO4)
7. concentrationconcentrated under reduced pressure
8. customto give a light-pink oil
9. customthe solid was recrystallized from methanol