反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 2 L Parr bottle were 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 (200 proof). 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. A viscous oil resulted, which was taken up in approximately 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. To the resulting suspension were added 300 ml of hexane. Filtration yielded 34 g (98%) of the expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride (Compound 14).
WORKUP
后处理
- customThe crude reaction mixture
- filtrationwas filtered through Celite™
- filtrationfilter agent
- customevaporated in vacuo
- customA viscous oil resulted
- stirringstirred at room temperature for several hours
- customThe expected 3-amino-1-chloro-3-methyl-2-pentanone hydrochloride crystallized as a white solid
- additionTo the resulting suspension were added 300 ml of hexane
- filtrationFiltration