反応式
C[O:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([S:9]([CH3:12])(=[O:11])=[O:10])[CH:4]=1>Br.C(O)(=O)C>[CH3:12][S:9]([C:5]1[CH:4]=[C:3]([OH:2])[CH:8]=[CH:7][CH:6]=1)(=[O:10])=[O:11]参加物
4
実験手順
1-Methoxy-3-(methylsulfonyl)benzene (300 mg, 1.61 mmol) was suspended in 1.6 mL aqueous hydrobromic acid (48% w/w) and 1.6 mL acetic acid. The mixture was heated under reflux for 24 hours. The reaction was cooled back to room temperature and concentrated. The residue was purified by column chromatography through a 40 gram biotage silica gel cartridge eluting with 40-70% ethyl acetate/hexanes (gradient) to give the product as white solid. LRMS calc: 172.0; obs: 173.2 (M+1).
後処理
- temperatureThe mixture was heated
- temperatureunder reflux for 24 hours
- concentrationconcentrated
- customThe residue was purified by column chromatography through a 40 gram biotage silica gel cartridge
- washeluting with 40-70% ethyl acetate/hexanes (gradient)
出典と根拠
- ORDレコード
- ord-11b48ec471dc4eb293cd2916ea000e55
- 出典データセット
- uspto-grants-2013_01
- 特許番号
- US08343990B2
関連ノート
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