HRID46814

反应详情

EQUATION

反应方程式

HRID 46814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. additionA mixture of 21.7 g
  2. customis hydrogenated at room temperature
  3. filtrationThe catalyst is filtered off
  4. washwashed with ethanol
  5. customare evaporated in vacuo
  6. dissolutionThe residue is dissolved in ethyl ether
  7. washwashed with water
  8. customdried
  9. filtrationfiltered
  10. additionthe filtrate treated with gaseous HCl
  11. filtrationThe resulting white solid is filtered
  12. customrecrystallized from ethanolethyl ether
  13. washwashed with water
  14. customdried
  15. filtrationfiltered
  16. additionthe filtrate treated with gaseous HCl
  17. filtrationThe resulting white solid is filtered
  18. customrecrystallized from ethanol-ethyl ether (1:1)