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Ethanone, 1-[4-fluoro-2-(methylamino)phenyl]-2-(methylsulfinyl)- → 1-(4-Fluoro-2-methylaminophenyl)-2-(methylthio)ethanone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethanone, 1-[4-fluoro-2-(methylamino)phenyl]-2-(methylsulfinyl)- | HCID 10059700 | — |
| 反応物 | Sodium Bisulfite | HCID 23665763 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-(4-Fluoro-2-methylaminophenyl)-2-(methylthio)ethanone | HCID 19978474 | — |
反応手順
A mixture of 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphinylethanone (100 g), prepared in a similar manner to that described in Example 1, sodium hydrogen sulphite (1 kg) and water (2.5 1) was stirred under nitrogen and heated at 90°-105° for 3 hours. The mixture was allowed to cool and then stood at ambient temperature for 72 hours. The mixture was extracted with dichloromethane (3×250 ml) and the combined extracts evaporated to give a solid product. Crystallisation from hexane gave 1-(4-fluoro-2-methylaminophenyl)-2-(methylthio)ethanone, m.p. 61.5°-63°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05011931 |
| 出典データセット | uspto-grants-1991_04 |
| ORD ID | ord-85d25843b6ee4496b0ee63ddc2cf790e |
| 出典メモ | uspto-grants-1991_04 |