HRID649182

反应详情

EQUATION

反应方程式

HRID 649182 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4.00 Grams of 3-methyl-8-(5-methoxy-2-benzimidazolyl)thio-5,6,7,8-tetrahydroquinoline was dissolved in 80 ml of dichloromethane, to this solution was added dropwise slowly at -10° C. a solution which was prepared by dissolving 2.37 g of meta-chloroperbenzoic acid (85%) in 30 ml of dichloromethane. After the dropwise solution was finished, the reaction mixture was stirred at -10° C. to -4° C. for 15 minutes. Water was added to the reaction mixture, then was made alkaline by adding sodium carbonate, then extracted with diethyl ether. The diethyl ether layer was washed with an aqueous solution saturated with sodium chloride, then was dried with anhydrous magnesium sulfate. The solvent was removed from the extract by evaporation, and was recrystallized from dichloromethane-diethyl ether to obtain 2.30 g of 3-methyl-8-(5-methoxy-2-benzimidazolyl)sulfinyl-5,6,7,8-tetrahydroquinoline in the form of white powdery crystals. Melting point: 114°-114.5° C. (decomposed).

WORKUP

后处理

  1. additionwas added dropwise slowly at -10° C. a solution which
  2. customwas prepared
  3. extractionextracted with diethyl ether
  4. washThe diethyl ether layer was washed with an aqueous solution saturated with sodium chloride
  5. dry with materialwas dried with anhydrous magnesium sulfate
  6. customThe solvent was removed from the
  7. extractionextract by evaporation
  8. customwas recrystallized from dichloromethane-diethyl ether