HRID1829738

反应详情

EQUATION

反应方程式

HRID 1829738 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 7.8 g (0.03 mole) of 2-(2,4,6-trimethylbenzylthio)-pyridine-N-oxide in 50 ml of chloroform were added, with stirring at less than 10° C., a mixture of 6 g (0.03 mole) of metachloroperbenzoic acid (85%) in 100 ml of chloroform. The mixture was stirred overnight at room temperature. The mixture was then washed with saturated sodium bicarbonate solution, the chloroform layer was separated and dried over sodium sulfate. The sodium sulfate was filtered off and the chloroform solution evaporated to leave a residue, which was crystallized from ethanol. The product was filtered off, and air-dried, melting point 164–166° C., yield 7.2 g. C, H, N, calculated for C15H17NO2S: % C=65.43, % H=6.22; % N=5.09. Found: % C=66.22; % H=6.63; % N=5.13.

WORKUP

后处理

  1. additionwere added
  2. stirringThe mixture was stirred overnight at room temperature
  3. washThe mixture was then washed with saturated sodium bicarbonate solution
  4. customthe chloroform layer was separated
  5. dry with materialdried over sodium sulfate
  6. filtrationThe sodium sulfate was filtered off
  7. customthe chloroform solution evaporated
  8. customto leave a residue, which
  9. customwas crystallized from ethanol
  10. filtrationThe product was filtered off
  11. customair-dried