HRID127287
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
The mixture of 14.6 g of 4-phenyl-1-(4-pyridyl)-piperidin-2,6-dione, 12.3 g of 10% palladium on carbon and 200 ml of glacial acetic acid is hydrogenated at 1.7 atm. and 100° for 8 hours. After cooling, the mixture is filtered, evaporated, the residue dissolved in the minimum amount of water and the solution basified with sodium carbonate. It is extracted with ethyl acetate, the extract evaporated and the residue crystallized by trituration with 75 ml of diethyl ether-hexane (3:1) and recrystallized from 50 ml of isopropanol to yield the 4-phenyl-1-(4-piperidinyl)-piperidin-2,6-dione nelting at 182°-189°; its p-methoxyphenyl analog melts at 127°-129°.
WORKUP
后处理
- temperatureAfter cooling
- filtrationthe mixture is filtered
- customevaporated
- dissolutionthe residue dissolved in the minimum amount of water
- extractionIt is extracted with ethyl acetate
- customthe extract evaporated
- customthe residue crystallized by trituration with 75 ml of diethyl ether-hexane (3:1)
- customrecrystallized from 50 ml of isopropanol