反应详情

温度

20 °C

Potassium carbonate (540 mg, 1.5 eq) and 3-piperidino-propylamine (420 mg, 1 eq) are added successively to 2,6-dichloro-3-nitropyridine (500 mg, 1 eq) in solution in toluene (10 ml). After stirring for 2 hours at a temperature of approximately 20° C., the mixture is concentrated under reduced pressure at 40° C. then water (20 ml) and dichloromethane (70 ml) are added. 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 solid obtained, by flash chromatography on silica gel (eluent: heptane/ethyl acetate 3:7 to 100% ethyl acetate), produces the expected compound in the form of a yellow solid (473 mg; 61% yield).

1. concentrationthe mixture is concentrated under reduced pressure at 40° C.
2. additionwater (20 ml) and dichloromethane (70 ml) are added
3. extractionAfter decantation and extractions
4. washthe combined organic phases are washed with salt water
5. dry with materialdried over Na2SO4
6. concentrationthen concentrated under reduced pressure at 40° C
7. customPurification of the solid
8. customobtained, by flash chromatography on silica gel (eluent: heptane/ethyl acetate 3:7 to 100% ethyl acetate)