反应详情

A mixture of 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide (430 mg, 1 eq, prepared according to Example A1), 3-piperidino-propylamine (212 mg, 1.1 eq) and potassium carbonate (365 mg, 2 eq) in acetonitrile (10 ml) is heated under reflux for 3 hours then concentrated under reduced pressure at 40° C. The residue is taken up in dichloromethane (50 ml) and water (20 ml). After decantation and extractions, the combined organic phases are washed with salt water, dried over Na2SO4 then concentrated under reduced pressure at 40° C. Purification of the residue by flash chromatography on silica gel (eluent: ethyl acetate 100%) produces the expected compound in the form of a yellow oil (460 mg; 78% yield).

1. temperatureis heated
2. temperatureunder reflux for 3 hours
3. concentrationthen concentrated under reduced pressure at 40° C
4. extractionAfter decantation and extractions
5. washthe combined organic phases are washed with salt water
6. dry with materialdried over Na2SO4
7. concentrationthen concentrated under reduced pressure at 40° C
8. customPurification of the residue by flash chromatography on silica gel (eluent: ethyl acetate 100%)