HRID1867367

反应详情

EQUATION

反应方程式

HRID 1867367 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1 g (4.52 mmol) (rac)-1-benzyl-3-hydroxymethyl-piperidin-4-ol (ca 1:1 diast mixture, Synthesis (1999), 11, 1937-1943) in 25 ml of MeOH was treated with a solution of HCl in dioxane (1.24 ml, 4 M in dioxane, 4.97 mmol) and 95 mg of Pd(OH)2/C (20%) and was stirred over H2-atmosphere for 16 h. After filtration, new catalyst was added (95 mg of Pd(OH)2/C (20%)) and stirred over H2-atmosphere for 2 days. After filtration, the solution was evaporated under reduced pressure to yield 0.66 g (86%) of the title compound as a ca 1:1 cis/trans mixture, MS: 132.3 (MH+).

WORKUP

后处理

  1. filtrationAfter filtration, new catalyst
  2. additionwas added (95 mg of Pd(OH)2/C (20%))
  3. stirringstirred over H2-atmosphere for 2 days
  4. filtrationAfter filtration
  5. customthe solution was evaporated under reduced pressure