HRID46668

反应详情

EQUATION

反应方程式

HRID 46668 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

600 ml. anhydrous pyridine, 100 g. crystallized quinidinone, and 300 ml. 25% solution of diisobutylaluminum hydride (DIBAH) in toluene were in a reaction vessel and the reaction was allowed to proceed until the reduction was completed as indicated by thin layer chromatography. The mixture was then heated under vacuum (25 mm Hg) to remove the pyridine. The reaction mixture was then treated with 750 ml. of a 50/50 mixture of water and ethanol, and after refluxing for 2 hours and cooling, 92.7 g. of quinidine base were obtained, exhibiting a melting point of 174.5° C.

WORKUP

后处理

  1. temperatureThe mixture was then heated under vacuum (25 mm Hg)
  2. customto remove the pyridine
  3. additionThe reaction mixture was then treated with 750 ml
  4. additionof a 50/50 mixture of water and ethanol
  5. temperatureafter refluxing for 2 hours
  6. temperaturecooling