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
A mixture of 21.7 g. (0.073 mole) of 3-tert.butyl-1-chloro-4-phenyl isoquinoline, 4.09 g. (0.073 mole) potassium hydroxide, 1.09 g 10% palladium on carbon and 1 liter of ethanol is hydrogenated at room temperature and 50 psi until 1 equivalent of hydrogen is absorbed. The catalyst is filtered off and washed with ethanol, combined ethanol portions are evaporated in vacuo. The residue is dissolved in ethyl ether, washed with water, dried, and filtered and the filtrate treated with gaseous HCl. The resulting white solid is filtered and recrystallized from ethanolethyl ether, washed with water, dried, and filtered and the filtrate treated with gaseous HCl. The resulting white solid is filtered and recrystallized from ethanol-ethyl ether (1:1) to give 3-tert.butyl-4-phenyl isoquinoline hydrochloride; m.p. 236°-238° C.
WORKUP
后处理
- additionA mixture of 21.7 g
- customis hydrogenated at room temperature
- filtrationThe catalyst is filtered off
- washwashed with ethanol
- customare evaporated in vacuo
- dissolutionThe residue is dissolved in ethyl ether
- washwashed with water
- customdried
- filtrationfiltered
- additionthe filtrate treated with gaseous HCl
- filtrationThe resulting white solid is filtered
- customrecrystallized from ethanolethyl ether
- washwashed with water
- customdried
- filtrationfiltered
- additionthe filtrate treated with gaseous HCl
- filtrationThe resulting white solid is filtered
- customrecrystallized from ethanol-ethyl ether (1:1)