反应详情

A solution of 3-dimethylaminomethylene-2′-(4-methoxybenzyloxy)-2,3,5,6-tetrahydro[1,3′]bipyridinyl-4-one (673 mg, 1.83 mmol) in ethanol (100 ml) was treated with guanidine carbonate (1.32 g, 7.33 mmol), followed by addition of sodium acetate trihydrate (1.99 g, 14.64 mmol) and the reaction mixture was refluxed for 21 hours. The solvent was removed in vacuo and the residue was partitioned between water and ethyl acetate. The separated organic layer was dried (MgSO4), filtered, and concentrated. Elution through a flash column (silica gel 60, 230-400 mesh, 6% methanol in EtOAc) gave the title compound as a light yellow, amorphous solid (477 mg, 72%).

1. temperaturethe reaction mixture was refluxed for 21 hours
2. customThe solvent was removed in vacuo
3. customthe residue was partitioned between water and ethyl acetate
4. dry with materialThe separated organic layer was dried (MgSO4)
5. filtrationfiltered
6. concentrationconcentrated
7. washElution through a flash column (silica gel 60, 230-400 mesh, 6% methanol in EtOAc)