HRID1598366

反应详情

EQUATION

反应方程式

HRID 1598366 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of crude 4-benzyl-2-phthalimidomethylmorpholine (64 g) in ethanol (500 ml) was added hydrazine monohydrate (18 ml, 0.57 mol) and the mixture was heated under reflux for 2 hours. After cooling, 10% aqueous sodium hydroxide (200 ml) was added to dissolve insolubles and the ethanol was distilled off under reduced pressure. The aqueous layer was extracted with chloroform (200 ml×3), the combined organic layer was dried over potassium carbonate and the solvent was distilled off to give crude 2-aminomethyl-4-benzylmorpholine (42.97 g). This compound was used for the subsequent reaction without purification.

WORKUP

后处理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 2 hours
  3. temperatureAfter cooling
  4. dissolutionto dissolve insolubles
  5. distillationthe ethanol was distilled off under reduced pressure
  6. extractionThe aqueous layer was extracted with chloroform (200 ml×3)
  7. dry with materialthe combined organic layer was dried over potassium carbonate
  8. distillationthe solvent was distilled off