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
- customThe crude reaction mixture
- filtrationwas filtered through Celite™
- customevaporated in vacuo
- customyielding a viscous oil, which
- stirringstirred at room temperature for several hours
- customThe expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid
- addition300 mL of hexane was added to the resulting suspension
- filtrationfiltered
출처 및 근거
- ORD 기록
- ord-b35b5640c43c4db797120639a758de49
- 출처 데이터셋
- uspto-grants-2000_10
- 특허 번호
- US06140362
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