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

HRID 363482

반응식

HRID 363482 반응식
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]

참가 물질

6

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-60141eb868aa4d0b8796f683a7c2e097
출처 데이터셋
uspto-grants-1999_02
특허 번호
US05874466

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