HRID8203

反应详情

EQUATION

反应方程式

HRID 8203 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Concentrated hydrochloric acid (0.35 mL) is added to a suspension of 1-(benzhydrylidene-amino)-4-(3-methoxy-phenyl)-pyrrolidin-2-one, (0.8 g, 2.16 mmol) in water (17 mL) and refluxed for one hour. The mixture is concentrated in vacuo and water azeotroped away using ethanol and toluene. The residue is dissolved in methanol (5 mL) and loaded on SCX resin (5 g). The resin is washed with methanol and 2 M solution of ammonia in methanol. Appropriate fractions are concentrated to yield the title compound, 402 mg (92%), as a white crystalline solid.

WORKUP

后处理

  1. temperaturerefluxed for one hour
  2. concentrationThe mixture is concentrated in vacuo and water
  3. customazeotroped away using ethanol and toluene
  4. dissolutionThe residue is dissolved in methanol (5 mL)
  5. washThe resin is washed with methanol and 2 M solution of ammonia in methanol
  6. concentrationAppropriate fractions are concentrated