Acetic Anhydride → 6-[(2-Oxopropyl)amino]pyridine-3-carboxylic acid
反応式
[CH3:1][NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][N:4]=1.[C:12](OC(=O)C)(=[O:14])[CH3:13]>>[C:12]([CH2:1][NH:2][C:3]1[CH:11]=[CH:10][C:6]([C:7]([OH:9])=[O:8])=[CH:5][N:4]=1)(=[O:14])[CH3:13]参加物
3
実験手順
A 1.5 g portion of 6-methylaminonicotinic acid in 20 ml of acetic anhydride was heated under reflux for 1.5 hours. After evaporation of the solvent under reduced pressure, the residue was dissolved with saturated aqueous sodium bicarbonate, and the aqueous layer was washed with ethyl acetate and then adjusted to pH 3 using concentrated hydrochloric acid. Then the aqueous layer was extracted with chloroform, the organic layer was washed and dried, and then the solvent was evaporated under reduced pressure to obtain 280 mg of the title compound as white crystals.
後処理
- temperatureunder reflux for 1.5 hours
- customAfter evaporation of the solvent under reduced pressure
- dissolutionthe residue was dissolved with saturated aqueous sodium bicarbonate
- washthe aqueous layer was washed with ethyl acetate
- extractionThen the aqueous layer was extracted with chloroform
- washthe organic layer was washed
- customdried
- customthe solvent was evaporated under reduced pressure
出典と根拠
- ORDレコード
- ord-959d8bb651d44dfabb5de79cbff7b980
- 出典データセット
- uspto-grants-2004_01
- 特許番号
- US06673799B1
反応ノート
読み込み中…