N-(3-Formyl-2-pyridinyl)-2,2-dimethylpropanamide → 3-Pyridinecarboxaldehyde, 2-amino-

HRID 228899

反応式

HRID 228899 の反応式
[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) to prepare a solution which was then stirred under reflux overnight. The reaction solution was cooled to room temperature, the reaction solution was washed with diethyl ether, and was neutralized with potassium carbonate powder. Diethyl ether was added thereto for extraction. The diethyl ether layer was dried over potassium carbonate. The solvent was removed by distillation under the reduced pressure, and 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

  1. customto prepare a solution which
  2. temperatureunder reflux overnight
  3. washthe reaction solution was washed with diethyl ether
  4. additionDiethyl ether was added
  5. extractionfor extraction
  6. dry with materialThe diethyl ether layer was dried over potassium carbonate
  7. customThe solvent was removed by distillation under the reduced pressure
  8. customthe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-460979f9aaea45399b0df40e80434104
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

関連ノート

読み込み中…