Methanol → Methyl 3-amino-2-fluorobenzoate
반응식
[NH2:1][C:2]1[C:3]([F:11])=[C:4]([CH:8]=[CH:9][CH:10]=1)[C:5]([OH:7])=[O:6].S(=O)(=O)(O)O.[CH3:17]O>>[CH3:17][O:6][C:5](=[O:7])[C:4]1[CH:8]=[CH:9][CH:10]=[C:2]([NH2:1])[C:3]=1[F:11]참가 물질
4
실험 절차
In a round bottom flask, 3-amino-2-fluoro-benzoic acid (71, 2.51 g, 16.2 mmol) is dissolved in 100 mL of methanol and 1 mL of concentrated sulfuric acid is added. The reaction is heated to reflux for 24 hours and an additional 1 mL of concentrated sulfuric acid is added. The reaction is heated to reflux another 20 hours, then extracted with ethyl acetate and saturated aqueous sodium chloride. The organic layer is isolated and washed with water, sodium bicarbonate, and brine, then dried with magnesium sulfate, and filtered. The filtrate is concentrated under vacuum to provide the desired compound (72, 2.688 g).
후처리
- temperatureThe reaction is heated
- temperatureto reflux for 24 hours
- temperatureThe reaction is heated
- temperatureto reflux another 20 hours
- extractionextracted with ethyl acetate and saturated aqueous sodium chloride
- customThe organic layer is isolated
- washwashed with water, sodium bicarbonate, and brine
- dry with materialdried with magnesium sulfate
- filtrationfiltered
- concentrationThe filtrate is concentrated under vacuum
출처 및 근거
- ORD 기록
- ord-3701941672854ff19d0a6b861aa08e80
- 출처 데이터셋
- uspto-grants-2014_03
- 특허 번호
- US08673928B2
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