Reaktionsgleichung
[C:1](Cl)(=[O:6])[CH2:2][C:3](Cl)=[O:4].[C:8]([CH2:11][C:12](=[O:14])[CH3:13])(=[O:10])[CH3:9]>>[C:8]([C:11]1[C:1]([OH:6])=[CH:2][C:3](=[O:4])[O:14][C:12]=1[CH3:13])(=[O:10])[CH3:9]Komponenten
3
Versuchsvorschrift
When 7.0 mL (72.0 mmol) of malonyl chloride was added to 7.0 mL (67.8 mmol) of acetylacetone, a violent exothermic reaction occurred to give a black solid within a few minutes. The solid was cooled to room temperature, washed with ether and then ethyl acetate, and filtered. The thus-obtained brown solid was recrystallized from ethyl acetate/methanol to give 1.75 g (10.4 mmol, 15.3%) of 5-acetyl-4-hydroxy-6-methyl-2-pyrone as brown crystals. The filtrates from washing and the recrystallized mother liquor were combined and concentrated; the residue was purified by silica gel column chromatography to give 2.87 g (17.1 mmol, 25.2%) of 5-acetyl-4-hydroxy-6-methyl-2-pyrone as orange crystals.
Aufarbeitung
- customa violent exothermic reaction
- customto give a black solid within a few minutes
- washwashed with ether
- filtrationethyl acetate, and filtered
- customThe thus-obtained brown solid was recrystallized from ethyl acetate/methanol
Quellen und Nachweise
- ORD-Eintrag
- ord-71cfa9d4f9044da782a2e89a0fc99d90
- Quelldatensatz
- uspto-grants-2001_04
- Patentnummer
- US06215016B1
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