Hydrochloric Acid → 4-Methylpentane-2,3-dione 2-oxime
Reaction equation
[CH3:1][CH:2]([C:4](=[O:7])[CH2:5][CH3:6])[CH3:3].Cl.[N:9](OCCC(C)C)=[O:10]>COC(C)(C)C.COCCOC>[CH3:1][CH:2]([CH3:3])[C:4](=[O:7])[C:5](=[N:9][OH:10])[CH3:6]Participants
6
[CH3:1][CH:2]([C:4](=[O:7])[CH2:5][CH3:6])[CH3:3].Cl.[N:9](OCCC(C)C)=[O:10]>COC(C)(C)C.COCCOC>[CH3:1][CH:2]([CH3:3])[C:4](=[O:7])[C:5](=[N:9][OH:10])[CH3:6]100 g (948 mmol) of 2-methylpentan-3-one were dissolved in 400 ml of tert-butyl methyl ether. 50 g (274 mmol) of solution of hydrochloride in ethylene glycol dimethyl ether (20%) were added. Subsequently, a solution of 117 g (949 mmol) isoamyl nitrite in 150 ml of tert-butyl methyl ether was added dropwise within 60 minutes. The solvent was removed fully under reduced pressure. The residue was taken up in 300 ml of n-heptane and concentrated again under reduced pressure. After 200 ml of n-heptane had been added, extraction was effected with 522 ml of sodium hydroxide solution (2 molar). After phase separation, the aqueous phase was washed with n-heptane. The aqueous phase was acidified by adding conc. hydrochloric acid. The product was isolated by filtration with suction, washed with water and dried at elevated temperature under reduced pressure.
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