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[CH2:1]([S:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)[CH3:2].S([O-])(O[O-])(=O)=[O:14].[K+].[K+].[OH2:21]>CO>[CH2:1]([S:3]([C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][CH:5]=1)(=[O:14])=[O:21])[CH3:2]참가 물질
5
실험 절차
To a stirring solution of 4-(ethylthio)benzoic acid (1 g, 5.5 mmol) in methanol (30 mL) at 0° C. under argon was added a solution of potassium peroxymonosulfate (6.8 g, 11 mmol) in water (30 mL). The resulted suspension was stirred at room temperature for 15 h. Methanol was evaporated under vacuum, the reaction mixture was diluted with water (30 mL), and the product was extracted with EtOAc (2×30 mL). The combined organic phase was washed with saturated aqueous NaCl, dried (MgSO4), filtered and concentrated under reduced pressure to obtain 910 mg of title compound as a white solid. HPLC/MS: retention time=1.695 min, [M+H]+=215.
후처리
- customMethanol was evaporated under vacuum
- additionthe reaction mixture was diluted with water (30 mL)
- extractionthe product was extracted with EtOAc (2×30 mL)
- washThe combined organic phase was washed with saturated aqueous NaCl
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-b72705c2182d4eceafbc4e79c2daa821
- 출처 데이터셋
- uspto-grants-2008_11
- 특허 번호
- US07452892B2
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