HRID29228

反应详情

EQUATION

反应方程式

HRID 29228 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of lithium aluminium hydride (3 g, 0.08 mols) in 350 ml of anhydrous ether is added with 0.5 g of 3-(2-hydroxy-5-methyl-phenyl)-N,N-diisopropyl-3-phenyl-propionamide in portions. The mixture is refluxed while stirring for 4 days. Afterwards, water is carefully added to destroy the lithium aluminium hydride excess, the mixture is acidified to pH 5 with acetic acid, the ether phase is separated and dried over sodium sulfate. The solvent is evaporated to obtain an oil which is purified by flash chromatography (eluent hexane-ethyl acetate 7:3). 0.1 g of tolterodine free base are obtained.

WORKUP

后处理

  1. temperatureThe mixture is refluxed
  2. customto destroy the lithium aluminium hydride excess
  3. customthe ether phase is separated
  4. dry with materialdried over sodium sulfate
  5. customThe solvent is evaporated
  6. customto obtain an oil which
  7. customis purified by flash chromatography (eluent hexane-ethyl acetate 7:3)