反应详情

To a slurry of sodium hydride (95%, 0.045 g, 1.8 mmol) in 10 mL anhydrous THF at 0° C. under an atmosphere of N2 was added diethyl malonate (0.32 g, 2.0 mmol) dropwise. The mixture was stirred for 30 minutes at ambient temperature, treated with the product from Example 24a (0.141 g, 0.3 mmol), heated at 110° C. for two hours, cooled and partitioned between EtOAc and water. The ethyl acetate layer washed with saturated brine, dried over sodium sulfate, filtered and concentrated giving the title compound as a yellow glass, (0.14 g, 84% yield).

1. temperatureheated at 110° C. for two hours
2. temperaturecooled
3. custompartitioned between EtOAc and water
4. washThe ethyl acetate layer washed with saturated brine
5. dry with materialdried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated