Methanol → Methyl 2-chloro-5-fluoronicotinate
反応式
[Cl:1][C:2]1[N:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].S(=O)(=O)(O)O.[OH-].[Na+].[CH3:19]O>>[Cl:1][C:2]1[N:10]=[CH:9][C:8]([F:11])=[CH:7][C:3]=1[C:4]([O:6][CH3:19])=[O:5]参加物
5
反応条件
- 温度
- 0 °C
実験手順
To a solution of 2-chloro-5-fluoronicotinic acid (5.2 g, 30 mmol) in methanol (20 ml) was added cone, sulfuric acid (0.5 ml) and the reaction mixture was stirred at reflux for 30 hours. The reaction mixture was cooled to 0° C. and 0.5 N sodium hydroxide solution was added to the mixture. The whole was extracted with diethylether. The organic phase was washed with brine, dried (sodium sulfate), and concentrated to afford 3.2 g (25%) of the title compound:
後処理
- temperatureat reflux for 30 hours
- extractionThe whole was extracted with diethylether
- washThe organic phase was washed with brine
- dry with materialdried (sodium sulfate)
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-a769b96ebc704cbe967caff54181e0ee
- 出典データセット
- uspto-grants-2011_12
- 特許番号
- US08084476B2
反応ノート
読み込み中…