HRID1638592

反应详情

EQUATION

反应方程式

HRID 1638592 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

1.5 Grams of 2-mercaptoimidazo[4,5-b]pyridine was dissolved in 50 ml of dimethylformamide, to this solution was added, under ice-cooled condition, 0.88 g of 60% sodium hydride (in oil), and the mixture was stirred at the same temperature for 30 minutes. Then, to this reaction mixture was added 2.2 g of 2-chloromethyl-3,5-dimethyl-4-methoxypyridine hydrochloride and the whole mixture was heated at 70° to 80° C. under stirring condition for 3 hours. After the reaction was completed, dimethylformamide was removed by evaporation, and to the residue thus obtained was added water, and then extracted with chloroform. The chloroform extract was washed with water, and dried with anhydrous magnesium sulfate. Chloroform was removed by evaporation, then the residue thus obtained was recrystallized from ethanol to obtain 1.3 g of 2-[(3,5-dimethyl-4-methoxy-2-pyridyl)methylthio]imidazo[4,5-b]pyridine in the form of white powdery crystals. Melting point: 186°-188° C.

WORKUP

后处理

  1. additionwas added, under ice-
  2. temperaturethe whole mixture was heated at 70° to 80° C.
  3. stirringunder stirring condition for 3 hours
  4. customdimethylformamide was removed by evaporation
  5. customto the residue thus obtained
  6. extractionextracted with chloroform
  7. extractionThe chloroform extract
  8. washwas washed with water
  9. dry with materialdried with anhydrous magnesium sulfate
  10. customChloroform was removed by evaporation
  11. customthe residue thus obtained
  12. customwas recrystallized from ethanol