反应 #933

ord-a610715a9a2049339b2b5008fb407eed

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

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

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.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US05723452uspto-grants-1998_03