반응 #935

ord-f52f628e55bf48349560d5f7350120df

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    추출The H2O solution was extracted with EtOAc
  2. 2
    건조After drying over MgSO4 and solvent removal
  3. 3
    기타the resultant crude product was purified by flash column chromatography on silica gel with methylene chloride as the eluent
  4. 4
    기타This resulted in 1.7 g of 2-fluoro-6-[(3-methoxyphenyl)sulfinyl]benzonitrile as a solid

실험 절차

To a solution of 2 g (7.7 mmol) of 2-fluoro-6-[(3-methoxyphenyl)thio]benzonitrile (Example 13) was added portionwise 1.6 g (9.3 mmol) of m-chloroperbenzoic acid. The resultant mixture was stirred for 24 h. Additional 0.16 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 eluent. This resulted in 1.7 g of 2-fluoro-6-[(3-methoxyphenyl)sulfinyl]benzonitrile as a solid: mp 103°-111° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05723452uspto-grants-1998_03