Hydrochloric Acid → 4-Methylpentane-2,3-dione 2-oxime

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.

1. customThe solvent was removed fully under reduced pressure
2. concentrationconcentrated again under reduced pressure
3. additionAfter 200 ml of n-heptane had been added
4. extractionextraction
5. customAfter phase separation
6. washthe aqueous phase was washed with n-heptane
7. additionby adding conc. hydrochloric acid
8. customThe product was isolated by filtration with suction
9. washwashed with water
10. customdried at elevated temperature under reduced pressure

ORD-Eintrag

ord-0779af3861ca42238d8739716743da4b

Quelldatensatz

uspto-grants-2009_06

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07544809B2