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m-Chloroperbenzoic acid → 2-Fluoro-6-[(3-methoxyphenyl)sulfinyl]benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | m-Chloroperbenzoic acid | HCID 70297 | — |
| 反応物 | 2-Fluoro-6-[(3-methoxyphenyl)thio]benzonitrile | HCID 10706406 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Fluoro-6-[(3-methoxyphenyl)sulfinyl]benzonitrile | HCID 10778773 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05723452 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-f52f628e55bf48349560d5f7350120df |
| 出典メモ | uspto-grants-1998_03 |