反应详情

A mixture of 3-fluoro-N,N-bis(3-methylbutyl)-4-nitrobenzamide (430 mg, 1 eq), 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 extraction, 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: heptane/ethyl acetate 1:1 to 100% ethyl acetate) 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 extraction
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: heptane/ethyl acetate 1:1 to 100% ethyl acetate)