反应详情

Magnesium methoxide (6% in MeOH, 530 mL) was added to a suspension of dehydroacetic acid (31 g) in methanol (600 mL) at room temperature. The reaction mixture was refluxed and stirred for 5 h. The solvent was removed and the residue dissolved in HCl 1M (1.5 L). The aqueous phase was extracted with EtOAc (2×750 mL) and then the solvent was evaporated under reduced pressure to give a yellow oil, which was filtered on a silica cartridge using dichloromethane as eluent. After the solvent removal, methyl 3,5-dioxohexanoate was obtained as a light yellow oil (19.9 g).

1. temperatureThe reaction mixture was refluxed
2. customThe solvent was removed
3. dissolutionthe residue dissolved in HCl 1M (1.5 L)
4. extractionThe aqueous phase was extracted with EtOAc (2×750 mL)
5. customthe solvent was evaporated under reduced pressure
6. customto give a yellow oil, which
7. filtrationwas filtered on a silica cartridge
8. customAfter the solvent removal