Methanol → Methyl 4-bromo-2-(methylsulfonyl)benzoate
반응식
[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=[O:7])=[C:4]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:3]=1.S(=O)(=O)(O)O.[CH3:20]O>>[Br:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([O:8][CH3:20])=[O:7])=[C:4]([S:11]([CH3:14])(=[O:13])=[O:12])[CH:3]=1참가 물질
4
실험 절차
A suspension of 4-bromo-2-(methylsulphonyl)benzoic acid (5.00 g; 17.9 mmol) in MeOH (100 ml) was treated with conc. sulphuric acid and the resulting mixture was heated at reflux for 5 days. The mixture was concentrated under reduced pressure, the residue was dissolved in EtOAc then washed with water, twice with NaHCO3 (sat) then with brine, dried on MgSO4, filtered and concentrated to give the title compound as a yellow solid (4.00 g, 72%).
후처리
- temperaturethe resulting mixture was heated
- temperatureat reflux for 5 days
- concentrationThe mixture was concentrated under reduced pressure
- dissolutionthe residue was dissolved in EtOAc
- washthen washed with water, twice with NaHCO3 (sat)
- dry with materialwith brine, dried on MgSO4
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-10fee52c43184a85a00800637e46a4c6
- 출처 데이터셋
- uspto-grants-2012_09
- 특허 번호
- US08273769B2
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