Methanol → Methyl 3-amino-2-fluorobenzoate
反応式
[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]参加物
4
実験手順
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).
後処理
- 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
出典と根拠
- ORDレコード
- ord-3701941672854ff19d0a6b861aa08e80
- 出典データセット
- uspto-grants-2014_03
- 特許番号
- US08673928B2
反応ノート
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