반응 #933
ord-a610715a9a2049339b2b5008fb407eed
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상세 조건
See reaction.notes.procedure_details.
후처리
- 1추출The H2O solution was extracted with EtOAc
- 2건조After drying over MgSO4 and solvent removal
- 3기타the resultant crude product was purified by flash column chromatography on silica gel with methylene chloride as the fluent
- 4기타This resulted in 1.15 g of 2-fluoro-6-[(3-methoxyphenyl)sulfonyl]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 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.