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

HRID 1602062Notes

Reaction equation

HRID 1602062 reaction equation
Cl.[NH2:2][C:3]([CH3:11])([CH2:9][CH3:10])[C:4](=[O:8])[CH:5](Cl)[Cl:6].C.C(O)C>C(OCC)(=O)C.[Pd]>[ClH:6].[NH2:2][C:3]([CH3:11])([CH2:9][CH3:10])[C:4](=[O:8])[CH2:5][Cl:6]

Participants

6

Procedure

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® filter agent 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.

Workup

  1. customThe crude reaction mixture
  2. filtrationwas filtered through Celite®
  3. filtrationfilter agent
  4. customevaporated in vacuo
  5. customyielding a viscous oil, which
  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. addition300 mL of hexane was added to the resulting suspension
  9. filtrationfiltered

Sources & evidence

ORD record
ord-bc5a864ce4bd4dbdb66ae768e838d6d0
Source dataset
uspto-grants-1999_11
Patent number
US05981435

Reaction notes

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