반응식
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]참가 물질
4
실험 절차
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).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-11b48ec471dc4eb293cd2916ea000e55
- 출처 데이터셋
- uspto-grants-2013_01
- 특허 번호
- US08343990B2
연결된 노트
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