反应详情

温度

90 °C

To a solution of ethyl 3-(2,6-dimethoxypyridin-3-yl)-3-oxopropanoate (500 mg, 1.97 mmol) in EtOH (4 mL) was added 2-aminoethanol (0.60 mL, 9.9 mmol) followed by acetic acid (0.63 mL, 9.9 mmol). The reaction mixture was heated to 90° C. for 16 hours, cooled to room temperature and concentrated in vacuo. The residue was partitioned between EtOAc and water. The organic layer was concentrated in vacuo and the crude material was purified by chromatography on silica eluting with 20-80% EtOAc/heptane to provide the title compound (573 mg, 98%) as a clear gum.

1. temperaturecooled to room temperature
2. concentrationconcentrated in vacuo
3. customThe residue was partitioned between EtOAc and water
4. concentrationThe organic layer was concentrated in vacuo
5. customthe crude material was purified by chromatography on silica eluting with 20-80% EtOAc/heptane