反应详情

Butanedioic acid, monomethyl ester (4.0 g, 30.3 mmole) and CDI (5.40 g, 33.3 mmole) were dissoled in anhydrous DMF (15 ml). After stirring the solution at room temperature for 3 hours, (1Z)—N′-hydroxy-2-phenylethanimidamide (5.0 g, 33.3 mmole) was added and the solution heated at 90° C. for 20 hours. After evaporation of solvent, the residue was dissoled in EtOAc. The organic phase was washed with water and brine, dried over Na2SO4. After filtration and evaporation of solvent, the residue was purified by flash chromatogarphy on silica gel eluted with EtOAc/Hexane (25/75). The purification gave 5.2 g (69.7%) of product as light yellowish oil. LCMS calculated for C13H15N2O3 (M+H): 247.1. Found 247.0.

1. temperaturethe solution heated at 90° C. for 20 hours
2. customAfter evaporation of solvent
3. washThe organic phase was washed with water and brine
4. dry with materialdried over Na2SO4
5. filtrationAfter filtration and evaporation of solvent
6. customthe residue was purified by flash chromatogarphy on silica gel
7. washeluted with EtOAc/Hexane (25/75)
8. customThe purification