HRID461972

反应详情

EQUATION

反应方程式

HRID 461972 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of N-cyclopentyloxyphthalimide (11 g), 100% hydrazine hydrate (2.6 g), and ethanol (30 ml) was heated under reflux for 5 minutes. Concentrated hydrochloride acid (6 ml) was added to the mixture, which was heated under reflux Water (20 ml) was added to the mixture, which was cooled to room temperature, and filtered. The filtrate was evaporated to dryness, ethanol (50 ml) was added to the residue, and a small amount of insoluble material was filtered off. The filtrate was evaporated to dryness, and the residue was recrystallised from ethanol/ether to give cyclopentyloxamine (6.28 g,) 96%), m.p. 156.9°.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 5 minutes
  3. temperaturewas heated under reflux Water (20 ml)
  4. additionwas added to the mixture, which
  5. filtrationfiltered
  6. customThe filtrate was evaporated to dryness, ethanol (50 ml)
  7. additionwas added to the residue
  8. filtrationa small amount of insoluble material was filtered off
  9. customThe filtrate was evaporated to dryness
  10. customthe residue was recrystallised from ethanol/ether