HRID1393137

反应详情

EQUATION

反应方程式

HRID 1393137 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

N-[3-(4-Pyridyl)propyl]phthalimide (67.1 g, 252 mmol) was mixed with methanol (504 ml) and hydrazine monohydrate (18.3 ml, 378 mmol), and the mixture was refluxed for three hours. The reaction mixture was allowed to stand, then an insoluble matter was filtered out, and the filtrate was concentrated under reduced pressure. Chloroform (1 liter) and a 4 N aqueous sodium hydroxide solution (500 ml) were added to the residue, layers were separated, and the organic layer was dried over sodium sulfate. The organic layer was concentrated under reduced pressure and then distilled under reduced pressure to give 20.5 g (60%) of the titled compound as a colorless oily matter.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for three hours
  2. filtrationan insoluble matter was filtered out
  3. concentrationthe filtrate was concentrated under reduced pressure
  4. additionChloroform (1 liter) and a 4 N aqueous sodium hydroxide solution (500 ml) were added to the residue, layers
  5. customwere separated
  6. dry with materialthe organic layer was dried over sodium sulfate
  7. concentrationThe organic layer was concentrated under reduced pressure
  8. distillationdistilled under reduced pressure