HRID649181

反应详情

EQUATION

反应方程式

HRID 649181 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

0.46 Gram of 2-chlorobenzimidazole, 0.2 g of thiourea and 10 ml of ethanol were mixed together and the mixture was refluxed for 2 hours. To this reaction mixture was added 0.62 g of 4-allyloxy-8-bromo-3-methyl-5,6,7,8-tetrahydroquinoline and 0.3 g of sodium hydroxide, then the whole reaction mixture was refluxed for 5 hours. After the reaction was completed, ethanol was removed by evaporation, and to the residue thus obtained was added water and then extracted with chloroform, and the chloroform extract was dried with anhydrous magnesium sulfate, and the chloroform was removed by evaporation. The residue thus obtained was purified by means of a silica gel column chromatography (eluent: methylene chloride/methanol=100/1) to obtain 0.5 g of 4-allyloxy-8-(2-benzimidazolyl)thio-3-methyl-5,6,7,8-tetrahydroquinoline in the form of light brown oily substance.

WORKUP

后处理

  1. temperaturethe mixture was refluxed for 2 hours
  2. customthe whole reaction mixture
  3. temperaturewas refluxed for 5 hours
  4. customethanol was removed by evaporation
  5. customto the residue thus obtained
  6. extractionextracted with chloroform
  7. extractionthe chloroform extract
  8. dry with materialwas dried with anhydrous magnesium sulfate
  9. customthe chloroform was removed by evaporation
  10. customThe residue thus obtained
  11. customwas purified by means of a silica gel column chromatography (eluent: methylene chloride/methanol=100/1)