HRID2051328

反应详情

EQUATION

反应方程式

HRID 2051328 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A suspension of 10.9 g (0.025 mol) of 8-chloro -1,2,3,4,5,6-hexahydro-4-(4-phthalimidobutyryl)benzo[f]-quinoline and 3.2 ml (0.065 mol) of hydrazine hydrate in 150 ml of ethanol is boiled at reflux temperature for 2 hours. The solution is concentrated, extracted with methylene chloride/water dried with sodium sulfate and the solvent is distilled in a vacuum. The residue is dissolved in 10 ml of 5.5N methanolic hydrochloric acid and precipitated with ether. Recrystallization from methanol/ether gives 4-(4-aminobutyryl)-8-chloro -1,2,3,4,5,6-hexahydrobenzo[f]quinoline hydrochloride as beige crystals with melting point 225°.

WORKUP

后处理

  1. temperatureat reflux temperature for 2 hours
  2. concentrationThe solution is concentrated
  3. extractionextracted with methylene chloride/water
  4. dry with materialdried with sodium sulfate
  5. distillationthe solvent is distilled in a vacuum
  6. dissolutionThe residue is dissolved in 10 ml of 5.5N methanolic hydrochloric acid
  7. customprecipitated with ether
  8. customRecrystallization from methanol/ether