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2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile → 2-[(3,5-Dimethylphenyl)sulfinyl]-6-fluorobenzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile | HCID 10848751 | — |
| 反応物 | Potassium hydroxy sulfite | HCID 23707502 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-[(3,5-Dimethylphenyl)sulfinyl]-6-fluorobenzonitrile | HCID 10730964 | 47% |
反応手順
2-[(3,5-Dimethylphenyl)thio]-6-fluorobenzonitrile (Example 18) (1.0 g, 3.9 mmol) was dissolved in 100 ml of methanol. A solution of OXONE®.dagger. (2.63 g, 4.3 mmol) in 15 ml of water was added dropwise with stirring. After stirring 1.5 h, the solid was removed by vacuum filtration and washed with 3×50 ml of methanol. The filtrate was concentrated to dryness and chromatographed on silica get (flash; Hex/EtOAc 2:1) to provide 0.5 g (47%) of 2-[(3,5-dimethylphenyl)sulfinyl]-6-fluorobenzonitrile: mp 146°-147° 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-6ddfb59c25f34fe781aa3d4f78fc3efa |
| 出典メモ | uspto-grants-1998_03 |