HRID1736402

反应详情

EQUATION

反应方程式

HRID 1736402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

In 300 ml of dimethylformamide were dissolved 89 g of 6-(3-chloropropoxy)-3,4-dihydrocarbostyril and 110 g of 1-(4-bromo-2-methylphenyl)-2-mercaptoimidazole. To the solution was slowly added 66.7 g of potassium carbonate at room temperature. The mixture was stirred at 80° C. for 2 hours to give rise to a reaction. After the completion of the reaction, the reaction mixture was extracted with ethyl acetate. The oily layer was washed with water thoroughly, washed with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent. The resulting brown oil was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1). The resulting crude crystals were recrystallized from ethanol to obtain 118 g of 6-{3-[1-(2-methyl-4-bromophenyl)-2-imidazolylthio]propoxy}-3,4-dihydrocarbostyril.

WORKUP

后处理

  1. customat room temperature
  2. customto give rise
  3. customto a reaction
  4. customAfter the completion of the reaction
  5. extractionthe reaction mixture was extracted with ethyl acetate
  6. washThe oily layer was washed with water thoroughly
  7. washwashed with an aqueous solution saturated with sodium chloride
  8. dry with materialdried with anhydrous magnesium sulfate
  9. distillationsubjected to distillation
  10. customto remove the solvent
  11. customThe resulting brown oil was purified by a silica gel column chromatography (eluant: chloroform/methanol=50/1)
  12. customThe resulting crude crystals were recrystallized from ethanol