HRID52136

反应详情

EQUATION

反应方程式

HRID 52136 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4-(2-Chloroethylthio)-2,3-dimethylpyridine-N-oxide (6 g) was dissolved in a mixed solution of dimethylformamide-toluene (1:1) and thereto were added potassium carbonate (4.3 g), potassium iodide (4.4 g) and morpholine (1.9 ml). The mixture was reacted at 50-55° C. for 12 hours. After the completion of the reaction, inorganic matters were filtered off and the solvent was distilled away. Water was added to the residue and the mixture was extracted with chloroform. After drying over anhydrous magnesium sulfate, the chloroform was distilled away and the obtained residue was purified by silica gel column chromatography to give 3.4 g of 2,3-dimethyl-4-(2-morpholinoethylthio)pyridine-N-oxide.

WORKUP

后处理

  1. customThe mixture was reacted at 50-55° C. for 12 hours
  2. customAfter the completion of the reaction, inorganic matters
  3. filtrationwere filtered off
  4. distillationthe solvent was distilled away
  5. additionWater was added to the residue
  6. extractionthe mixture was extracted with chloroform
  7. dry with materialAfter drying over anhydrous magnesium sulfate
  8. distillationthe chloroform was distilled away
  9. customthe obtained residue was purified by silica gel column chromatography