反应详情

温度

75 °C

To a suspension of 0.598 g (4.86 mmol) of 3-amino-4,6-dimethylpyridazine in 10 mL of CH2Cl2 in a high pressure vessel was added 0.941 g (1.27 mL; 7.28 mmol) of diisopropylethylamine and 1.301 g (7.28 mmol) of ethyl a-chloropropionylacetate. The reaction mixture was equipped with a magnetic stir bar, tightly sealed, then heated and stirred in an oil bath at 75° C. for 16 hours. The flask was then cooled to room temperature, opened and the reaction mixture was evaporated in vacuo. The residue was partitioned between EtOAc and water, and the organic layer was separated. The organic layer was washed with brine, dried (MgSO4), filtered and evaporated. The residual brown solid was purified on a silica gel flash chromatography column eluted with 50% EtOAc-hexane. Combination of the purified fractions and evaporation in vacuo afforded 0.874 g (73%) of the title compound.

1. customThe reaction mixture was equipped with a magnetic stir bar
2. customtightly sealed
3. temperatureheated
4. temperatureThe flask was then cooled to room temperature
5. customthe reaction mixture was evaporated in vacuo
6. customThe residue was partitioned between EtOAc and water
7. customthe organic layer was separated
8. washThe organic layer was washed with brine
9. dry with materialdried (MgSO4)
10. filtrationfiltered
11. customevaporated
12. customThe residual brown solid was purified on a silica gel flash chromatography column
13. washeluted with 50% EtOAc-hexane
14. customCombination of the purified fractions and evaporation in vacuo