HRID837

反应详情

EQUATION

反应方程式

HRID 837 的结构方程式

PROCEDURE

实验过程

To a solution of 2 g (7.7 mmol) of 2-fluoro-6-[(3-methoxyphenyl)thio]benzonitrile (Example 13) was added 2.93 g (17 mmol) of m-chloroperbenzoic acid. The resultant mixture was stirred for 24 h. Additional 0.29 g of m-chloroperbenzoic acid was added and the resultant mixture was stirred for 15 min. Excess sodium bisulfite was added, followed by water. The H2O solution was extracted with EtOAc. After drying over MgSO4 and solvent removal, the resultant crude product was purified by flash column chromatography on silica gel with methylene chloride as the fluent. This resulted in 1.15 g of 2-fluoro-6-[(3-methoxyphenyl)sulfonyl]benzonitrile as a solid: mp 113°-117° C.

WORKUP

后处理

  1. extractionThe H2O solution was extracted with EtOAc
  2. dry with materialAfter drying over MgSO4 and solvent removal
  3. customthe resultant crude product was purified by flash column chromatography on silica gel with methylene chloride as the fluent
  4. customThis resulted in 1.15 g of 2-fluoro-6-[(3-methoxyphenyl)sulfonyl]benzonitrile as a solid