HRID270043

反应详情

EQUATION

反应方程式

HRID 270043 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A stirred solution of ethyl 1-benzyl-4-(2-fluorobenzyl)piperidine-4-carboxylate (1.85 g, 5.2 mmol) in diethyl ether was cooled on ice/sodium chloride. Lithium aluminium hydride (5.8 mL, 1.0 M in diethyl ether) was added drop wise. After stirring at room temperature for 2 hrs the mixture was re-cooled on ice, quenched with water/sodium hydroxide (10%) and stirred at room temperature for 1 hrs. The solids were filtered off, and the organic layer was dried over disodium sulphate, filtrated and concentrated. The crude material was purified on silica (dichloromethane/ethanol) to give 1.0 g (61%) the subtitle compound.

WORKUP

后处理

  1. temperaturewas re-cooled on ice
  2. customquenched with water/sodium hydroxide (10%)
  3. stirringstirred at room temperature for 1 hrs
  4. filtrationThe solids were filtered off
  5. dry with materialthe organic layer was dried over disodium sulphate
  6. filtrationfiltrated
  7. concentrationconcentrated
  8. customThe crude material was purified on silica (dichloromethane/ethanol)