Methanol → Methyl 3-bromobenzoate
반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].[CH3:11]O>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([O:7][CH3:11])=[O:6]참가 물질
4
실험 절차
Part A: 3-Bromobenzoic acid (1.1 g, 5.47 mmol) was dissolved in methanol (20 ml) in a 50 ml flask. Concentrated sulfuric acid (2 drops) was added and the mixture was refluxed under nitrogen for ten hours then concentrated under reduced pressure. The residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml). The organic material was separated, dried (MgSO4) and concentrated under reduced pressure. The residue was flushed through silica gel with hexane/ethyl acetate (3:1), and concentrated which provided methyl 3-bromobenzoate (1.0 g, 85%).
후처리
- temperaturethe mixture was refluxed under nitrogen for ten hours
- concentrationthen concentrated under reduced pressure
- additionThe residue was mixed with dichloromethane (20 ml) and saturated sodium bicarbonate solution (10 ml)
- customThe organic material was separated
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
- customThe residue was flushed through silica gel with hexane/ethyl acetate (3:1)
- concentrationconcentrated which
출처 및 근거
- ORD 기록
- ord-02beae4f681d488aae48056e2215c553
- 출처 데이터셋
- uspto-grants-1997_04
- 특허 번호
- US05622937
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