反応式
ClC1C=C(C=CC=1)C(OO)=[O:6].[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](=[O:24])[CH2:20][S:21]([CH3:23])=[O:22])=[C:15]([NH:25][CH3:26])[CH:14]=1.C(=O)([O-])O.[Na+]>ClCCl>[F:12][C:13]1[CH:18]=[CH:17][C:16]([C:19](=[O:24])[CH2:20][S:21]([CH3:23])(=[O:6])=[O:22])=[C:15]([NH:25][CH3:26])[CH:14]=1参加物
実験手順
A solution of 3-chloroperoxybenzoic acid (8.29 g) in dichloromethane (200 ml) was added to a solution of 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphinylethanone (10.0 g), prepared in a similar manner to that described in Example 1, in dichloromethane (175 ml) over a period of 7 minutes whilst maintaining the temperature below 30°. The mixture was stirred at ambient temperature for 2 hours, saturated aqueous sodium hydrogen carbonate solution (244 ml) was added and the mixture stirred at ambient temperature for a further 2 hours. The dichloromethane layer was isolated and the aqueous layer extracted with dichloromethane (2×60 ml). The organic phases were combined, dried (magnesium sulphate) and evaporated in vacuo to give a solid which was crystallised from acetone to give 1-(4-fluoro-2-methylaminophenyl)-2-methylsulphonylethanone, m.p. 143.5°-145°.
後処理
- customprepared in a similar manner to that
- temperaturewhilst maintaining the temperature below 30°
- stirringthe mixture stirred at ambient temperature for a further 2 hours
- extractionthe aqueous layer extracted with dichloromethane (2×60 ml)
- dry with materialdried (magnesium sulphate)
- customevaporated in vacuo
- customto give a solid which
- customwas crystallised from acetone
出典と根拠
- ORDレコード
- ord-51121a7ad8924ca2a0d0378ab6f5a30e
- 出典データセット
- uspto-grants-1991_04
- 特許番号
- US05011931
関連ノート
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