反应详情

Ethyl 2-chloro-4-methyl-3-oxopentanoate (1.36 g, 7.09 mmol) was added to an ethanol (20 ml) solution of the compound (1.94 g, 5.45 mmol) obtained in Step 11 above at room temperature and the resulting mixture was heated to reflux for 16 hours. The reaction mixture was returned to room temperature and the reaction solvent was evaporated under reduced pressure. The residue obtained was diluted with ethyl acetate and the organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue obtained was purified by silica gel column chromatography [n-hexane:ethyl acetate=3:1 (v/v)] to give the title compound (2.06 g, 76%) as a colorless solid.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux for 16 hours
3. customwas returned to room temperature
4. customthe reaction solvent was evaporated under reduced pressure
5. customThe residue obtained
6. washthe organic layer was washed with saturated aqueous sodium bicarbonate solution and saturated brine
7. dry with materialdried over anhydrous magnesium sulfate
8. customThe solvent was evaporated under reduced pressure
9. customthe residue obtained
10. customwas purified by silica gel column chromatography [n-hexane:ethyl acetate=3:1 (v/v)]