Water → 2,6-Difluoro-nicotinic acid methyl ester
反応式
[F:1][C:2]1[N:10]=[C:9]([F:11])[CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.O.[C:18](=O)([O-])[O-].[K+].[K+]>CO>[CH3:18][O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][C:9]([F:11])=[N:10][C:2]=1[F:1]参加物
6
実験手順
To 2,6-difluoro-nicotinic acid (59, 5.60 g, 0.0352 mol) in methanol (60.0 mL) was added concentrated sulfuric acid (1.0 mL, 0.019 mol). The reaction was heated to reflux overnight, then poured into water, basified with 1M potassium carbonate to pH around 9, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate and concentrated to give a yellow oil (60, 3.5 g, 57.0%).
後処理
- temperatureThe reaction was heated
- temperatureto reflux overnight
- extractionextracted with ethyl acetate
- dry with materialThe organic layer was dried over anhydrous sodium sulfate
- concentrationconcentrated
- customto give a yellow oil (60, 3.5 g, 57.0%)
出典と根拠
- ORDレコード
- ord-457d5bb45a014f8c8eb941300a3b354c
- 出典データセット
- uspto-grants-2014_05
- 特許番号
- US08722702B2
反応ノート
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