反応式
[CH:1]([C:3]1[C:4]([NH:9]C(=O)C(C)(C)C)=[N:5][CH:6]=[CH:7][CH:8]=1)=[O:2]>Cl>[NH2:9][C:4]1[C:3]([CH:1]=[O:2])=[CH:8][CH:7]=[CH:6][N:5]=1参加物
3
実験手順
N-(3-Formyl-pyridin-2-yl)-2,2-dimethyl-propionamide (9.68 g) was dissolved in 3 N hydrochloric acid (140 ml), and the solution was stirred under reflux overnight. The reaction solution was cooled to room temperature, was then washed with diethyl ether, and was neutralized with potassium carbonate powder. Diethyl ether was added thereto, and the mixture was extracted. The diethyl ether layer was dried over potassium carbonate, and the solvent was removed by distillation under the reduced pressure. The residue was purified by column chromatography using acetone-chloroform to give 2-amino-pyridine-3-carbaldehyde (5.03 g, yield 88%).
後処理
- temperatureunder reflux overnight
- washwas then washed with diethyl ether
- additionDiethyl ether was added
- extractionthe mixture was extracted
- dry with materialThe diethyl ether layer was dried over potassium carbonate
- customthe solvent was removed by distillation under the reduced pressure
- customThe residue was purified by column chromatography
出典と根拠
- ORDレコード
- ord-ea5931a6b4484995b780c9630b52eb4d
- 出典データセット
- uspto-grants-2009_07
- 特許番号
- US07560558B2
関連ノート
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