Methane → 3-Amino-1-chloro-3-methylpentan-2-one hydrochloride

In a 2 L Parr bottle were placed 41 g of 3-amino-1,1-dichloro-3-methyl-2-pentanone hydrochloride, 0.8 g of 10% palladium over charcoal and 400 ml of ethanol (200 proof). The resulting mixture was shaken in a Parr apparatus at 50 psi for 3 hours. The crude reaction mixture was filtered through Celite™ filter agent and evaporated in vacuo. A viscous oil resulted, which was taken up in approximately 400 ml of ethyl acetate and stirred at room temperature for several hours. The expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid. To the resulting suspension were added 300 ml of hexane. Filtration yielded 34 g (98%) of the expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride (Compound 14).

1. customThe crude reaction mixture
2. filtrationwas filtered through Celite™
3. filtrationfilter agent
4. customevaporated in vacuo
5. customA viscous oil resulted
6. stirringstirred at room temperature for several hours
7. customThe expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid
8. additionTo the resulting suspension were added 300 ml of hexane
9. filtrationFiltration

ORD-Eintrag

ord-bfe75ec575e94cd696b03ae05edf33da

Quelldatensatz

uspto-grants-1999_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US05929098