HRID2308985

反应详情

EQUATION

反应方程式

HRID 2308985 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-[3-(N-phenyl-N-pyrid-2-ylamino)-propyl]phthalimide, (3.1 g) and conc. hydrochloric acid (30 ml) were heated under reflux for 21 hr. Phthalic acid was filtered off on cooling and the solvent was evaporated from the filtrate. The residue was dissolved in water and the solution extracted at pH 1 with chloroform. The pH was raised to pH 13 (NaOH) and the solution extracted again with ether. The ether extracts were dried (K2CO3) and the ether was evaporated to give 2-[N-(3-aminopropyl)-N-phenylamino]pyridine, 1.84 g as an oil.

WORKUP

后处理

  1. temperaturewere heated
  2. temperatureunder reflux for 21 hr
  3. filtrationPhthalic acid was filtered off
  4. temperatureon cooling
  5. customthe solvent was evaporated from the filtrate
  6. dissolutionThe residue was dissolved in water
  7. extractionthe solution extracted at pH 1 with chloroform
  8. temperatureThe pH was raised to pH 13 (NaOH)
  9. extractionthe solution extracted again with ether
  10. dry with materialThe ether extracts were dried (K2CO3)
  11. customthe ether was evaporated