反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([OH:11])=[O:10])[CH:5]=[N:6][CH:7]=1.[CH2:12](O)[CH3:13]>S(=O)(=O)(O)O>[Br:1][C:2]1[CH:3]=[C:4]([CH2:8][C:9]([O:11][CH2:12][CH3:13])=[O:10])[CH:5]=[N:6][CH:7]=1参加物
4
実験手順
5.0 g (23.1 mmol) of (5-bromopyridin-3-yl)acetic acid in 30 ml of ethanol and 25 drops of conc. sulfuric acid are stirred at boiling point for 16 h. For work-up, the reaction mixture is concentrated under reduced pressure, the residue is taken up in ethyl acetate and washed repeatedly with semiconcentrated sodium bicarbonate solution, the organic phase is dried over sodium sulfate, the drying agent is filtered off, the solvent is removed completely on a rotary evaporator and the product is dried under reduced pressure for 16 h.
後処理
- customfor 16 h
- concentrationFor work-up, the reaction mixture is concentrated under reduced pressure
- washwashed repeatedly with semiconcentrated sodium bicarbonate solution
- dry with materialthe organic phase is dried over sodium sulfate
- filtrationthe drying agent is filtered off
- customthe solvent is removed completely on a rotary evaporator
- customthe product is dried under reduced pressure for 16 h.
出典と根拠
- ORDレコード
- ord-e24430d98d0a4aaf9fb307533163ce10
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08524699B2
関連ノート
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