HRID1594628

反应详情

EQUATION

反应方程式

HRID 1594628 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Hydroxy4-(4-methylbenzyl)piperidine hydrochloride. A mixture of 1-benzyl-4-(4-methylbenzyl)-4-hydroxypiperidine (2.8 g, 9.5 mmol) and 700 mg of 10% Pd/C in 100 mL of 95% ethanol was hydrogenated at 50 psi for overnight. The catalyst was removed through a short column of celite (10 g) and washed with methanol (3×15 mL). To the filtrate was added 12 mL of 1M HCl in methanol. Evaporation of methanol gave a residue, to which was added 30 mL of ether. The mixture was stirred at rt for 2 days. A white solid was collected by filtration, giving 2.1 g (92%) of the title product: mp 183-185° C.

WORKUP

后处理

  1. customThe catalyst was removed through a short column of celite (10 g)
  2. washwashed with methanol (3×15 mL)
  3. additionTo the filtrate was added 12 mL of 1M HCl in methanol
  4. customEvaporation of methanol
  5. customgave a residue
  6. filtrationA white solid was collected by filtration