تفاعل #935

ord-f52f628e55bf48349560d5f7350120df

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

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

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05723452uspto-grants-1998_03