反应详情

温度

100 °C

Methyl-4-hydrazinylbenzoate hydrochloride (1 equiv.) and 1-methylpiperidin-4-one HCl (0.76-1.4 equiv.) are taken aqueous HCl and heated at 100° C. overnight (the product was detected by LCMS). The reaction mixture is concentrated and refluxed (90° C.) in methanolic HCl overnight (product was detected by LCMS and TLC). The reaction mixture is concentrated and basified with aqueous NaHCO3 solution and extracted with EtOAc. The crude product is crystallized in DCM and ether and hexane.

1. concentrationThe reaction mixture is concentrated
2. temperaturerefluxed (90° C.) in methanolic HCl overnight (product was detected by LCMS and TLC)
3. concentrationThe reaction mixture is concentrated
4. extractionextracted with EtOAc
5. customThe crude product is crystallized in DCM