HRID1088814

反应详情

EQUATION

反应方程式

HRID 1088814 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

8-Carboxythiomethyl-1-methyl-1,2,3,4-tetrahydroquinoline hydrochloride (27.9 g) and 5-methoxy-o-phenylenediamine (13.8 g) in 4N hydrochloric acid (100 ml) were refluxed for 40 minutes. The reaction mixture was cooled, neutralized with aqueous ammonia and extracted with chloroform. After drying the extract, the solvent was distilled off under reduced pressure and the resulting residue was purified by silica gel column chromatography [eluent:n-hexane-ethyl acetate (4:1)] to give 8-(5-methoxy-2-benzimidazolyl)thiomethyl-1-methyl-1,2,3,4-tetrahydroquinoline (5.0 g).

WORKUP

后处理

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with chloroform
  3. customAfter drying the extract
  4. distillationthe solvent was distilled off under reduced pressure
  5. customthe resulting residue was purified by silica gel column chromatography [eluent:n-hexane-ethyl acetate (4:1)]