反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH2:9][S:10]([CH3:12])=O)=[C:4]([NH:14][CH3:15])[CH:3]=1.S([O-])(O)=O.[Na+]>O>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH2:9][S:10][CH3:12])=[C:4]([NH:14][CH3:15])[CH:3]=1参加物
4
実験手順
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°.
後処理
- customprepared in a similar manner to that
- temperatureheated at 90°-105° for 3 hours
- temperatureto cool
- extractionThe mixture was extracted with dichloromethane (3×250 ml)
- customthe combined extracts evaporated
- customto give a solid product
- customCrystallisation from hexane
出典と根拠
- ORDレコード
- ord-fbebcd8fb6b94d05baa7770ec53116d7
- 出典データセット
- uspto-grants-1992_01
- 特許番号
- US05079264
関連ノート
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