HRID977628

反应详情

EQUATION

反应方程式

HRID 977628 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 1.04 g of 2,2-bisfluoromethyl-6-iodo-4-(2-pyridyl)-2H-1-benzopyran and 20 ml of methylene chloride was added 0.78 g of m-chloroperbenzoic acid (70%) with stirring under ice-cooling. The mixture was stirred under ice-cooling for 1 hour and then stirred at room temperature for 25 hours. Potassium carbonate solution was added thereto and the mixture was extracted with methylene chloride. The organic layer was washed with water and dried. The solvent was distilled off and the resultant residue was purified using silica gel column chromatography (developing solution, MeOH:CH2Cl2 =1:99) to obtain 0.25 g of oily 2-(2,2-bisfluoromethyl-6-iodo-2H-1-benzopyran-4-yl)pyridine N-oxide represented by the following formula.

WORKUP

后处理

  1. temperaturecooling
  2. stirringThe mixture was stirred under ice-
  3. temperaturecooling for 1 hour
  4. stirringstirred at room temperature for 25 hours
  5. extractionthe mixture was extracted with methylene chloride
  6. washThe organic layer was washed with water
  7. customdried
  8. distillationThe solvent was distilled off
  9. customthe resultant residue was purified