反応式
[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10][C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[CH:12]=2)[C:3]=1[C:4]#[N:5].ClC1C=CC=C(C(OO)=[O:27])C=1.S(=O)(O)[O-].[Na+].[OH2:35]>>[F:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([S:10]([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([O:17][CH3:18])[CH:12]=2)(=[O:27])=[O:35])[C:3]=1[C:4]#[N:5]参加物
5
実験手順
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.
後処理
- extractionThe H2O solution was extracted with EtOAc
- dry with materialAfter drying over MgSO4 and solvent removal
- customthe resultant crude product was purified by flash column chromatography on silica gel with methylene chloride as the fluent
- customThis resulted in 1.15 g of 2-fluoro-6-[(3-methoxyphenyl)sulfonyl]benzonitrile as a solid
出典と根拠
- ORDレコード
- ord-a610715a9a2049339b2b5008fb407eed
- 出典データセット
- uspto-grants-1998_03
- 特許番号
- US05723452
関連ノート
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