HRID2051328
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux temperature for 2 hours
- concentrationThe solution is concentrated
- extractionextracted with methylene chloride/water
- dry with materialdried with sodium sulfate
- distillationthe solvent is distilled in a vacuum
- dissolutionThe residue is dissolved in 10 ml of 5.5N methanolic hydrochloric acid
- customprecipitated with ether
- customRecrystallization from methanol/ether