反应详情

温度

25 °C

To a suspension of the product of step 1 in DCM at 0° C., DIPEA (4 eqv) was added slowly and stirred for 30 minutes at 25° C. The reaction mixture was cooled again to 0° C. and acetyl chloride (1.1 eqv) was added slowly. The resulting mixture was stirred at 25° C. for 16 hrs before being quenched by addition of saturated aqueous NaHCO3. The aqueous layer was back extracted three times with DCM. The combined organics were washed with H2O, dried (Na2SO4), filtered and evaporated. The residue was purified by SiO2 flash chromatography to give racemic 1-acetyl-3-methyl-piperidin-4-one (94% over two steps).

1. temperatureThe reaction mixture was cooled again to 0° C.
2. stirringThe resulting mixture was stirred at 25° C. for 16 hrs
3. custombefore being quenched by addition of saturated aqueous NaHCO3
4. extractionThe aqueous layer was back extracted three times with DCM
5. washThe combined organics were washed with H2O
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. customevaporated
9. customThe residue was purified by SiO2 flash chromatography