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

HRID 370026ノート

反応式

HRID 370026 の反応式
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]

参加物

6

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b35b5640c43c4db797120639a758de49
出典データセット
uspto-grants-2000_10
特許番号
US06140362

反応ノート

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