反应详情

温度

25 °C

A solution of the product of Example 3H (25.4 mmol) in ethanol (50 mL) was treated with ethyl bromopyruvate (3 mL, 23.9 mmol) and molecular sieves (10 g, 3 Å), heated at reflux for 16 hours, cooled to 25° C., filtered and concentrated. The concentrate was partitioned between ethyl acetate and saturated NaHCO3, and the organic phase was washed with brine, dried over MgSO4, filtered and concentrated. The residue was chromatographed on silica gel eluting with 0-25% ethyl acetate in dichloromethane to give the title compound (1.98 g, 33% yield).

1. temperatureheated
2. temperatureat reflux for 16 hours
3. filtrationfiltered
4. concentrationconcentrated
5. customThe concentrate was partitioned between ethyl acetate and saturated NaHCO3
6. washthe organic phase was washed with brine
7. dry with materialdried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe residue was chromatographed on silica gel eluting with 0-25% ethyl acetate in dichloromethane