N-bromobutanimide → Methyl 3-bromo-5-fluoro-4-hydroxybenzoate
반응식
[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:9]=[CH:8][C:7]([OH:10])=[C:6]([F:11])[CH:5]=1.[Br:13]N1C(=O)CCC1=O>C1COCC1.C(OCC)(=O)C>[CH3:1][O:2][C:3](=[O:12])[C:4]1[CH:5]=[C:6]([F:11])[C:7]([OH:10])=[C:8]([Br:13])[CH:9]=1참가 물질
5
실험 절차
To a solution of 3-fluoro-4-hydroxybenzoic acid methyl ester (1.0 g) in THF (10 mL) was added N-bromosuccinimide (1.26 g) under ice-cooling, and the mixture was stirred at room temperature for 2 hours The reaction solution was diluted with ethyl acetate, washed successively with saturated aqueous sodium bicarbonate and saturated brine, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography on silica gel (hexane:ethyl acetate=3:1, v/v) to give the title compound (1.16 g). (In the above, THF is tetrahydrofuran)
후처리
- temperaturecooling
- washwashed successively with saturated aqueous sodium bicarbonate and saturated brine
- dry with materialdried over anhydrous sodium sulfate
- concentrationconcentrated
- customThe residue was purified by column chromatography on silica gel (hexane
출처 및 근거
- ORD 기록
- ord-228cbbd811a94f878fcb2f5bc1593217
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08101774B2
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