HRID981097

反应详情

EQUATION

反应方程式

HRID 981097 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

17.3 g (58 mmol) of crude trans-1-benzyl-3-benzylmethylamino-4-hydroxy-pyrrolidine in 80 ml of absolute tetrahydrofuran are added dropwise to 2.8 g (93.3 mmol) of 80% strength sodium hydride in 40 ml of absolute tetrahydrofuran and the mixture is heated under reflux at the same time. When the evolution of hydrogen has ended, 8.7 g (61 mmol) of methyl iodide are added dropwise and the mixture is then heated under reflux overnight. It is poured into ice-water and extracted with toluene, the extracts are dried with K2CO3, and concentrated and the residue is distilled.

WORKUP

后处理

  1. temperaturethe mixture is heated
  2. temperatureunder reflux at the same time
  3. temperaturethe mixture is then heated
  4. temperatureunder reflux overnight
  5. extractionextracted with toluene
  6. dry with materialthe extracts are dried with K2CO3
  7. concentrationconcentrated
  8. distillationthe residue is distilled