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

In a 2 L Parr™ bottle was 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. The resulting mixture was shaken in a Parr™ apparatus at 50 psi for 3 hours. The crude reaction mixture was filtered through Celite™ and evaporated in vacuo yielding a viscous oil, which was taken in 300 to 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; 300 mL of hexane was added to the resulting suspension and filtered yielding 34 g (98%) of the expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride.

1. customThe crude reaction mixture
2. filtrationwas filtered through Celite™
3. customevaporated in vacuo
4. customyielding a viscous oil, which
5. stirringstirred at room temperature for several hours
6. customThe expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid
7. addition300 mL of hexane was added to the resulting suspension
8. filtrationfiltered

ORD record

ord-60141eb868aa4d0b8796f683a7c2e097

Source dataset

uspto-grants-1999_02

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05874466