Hydrochloric Acid → 3-Aminopicolinic acid

HRID 2386974

反応式

HRID 2386974 の反応式
[N+:1]([C:4]1[C:5]([C:10]([OH:12])=[O:11])=[N:6][CH:7]=[CH:8][CH:9]=1)([O-])=O.C(=O)([O-])O.[Na+].[H][H].Cl>O.[Pd]>[NH2:1][C:4]1[C:5]([C:10]([OH:12])=[O:11])=[N:6][CH:7]=[CH:8][CH:9]=1

参加物

7

実験手順

3-nitropyridine-2-carboxylic acid (2.72 g, 16.2 mmol) and sodium hydrogencarbonate (1.34 g, 16.2 mmol) were dissolved in distilled water (20 mL), and the atmosphere in the system was replaced by nitrogen. After adding 10% palladium charcoal (1.72 g), the atmosphere in the system was replaced by hydrogen, and the mixture stirred at room temperature for 50 hours. 1N hydrochloric acid aqueous solution was added, and the pH of the reaction solution was adjusted to weak acidity. The solvent was distilled off under reduced pressure, a small amount of ethanol and ethyl acetate were added to the residue, and the precipitate produced was filtered off. The filtrate was concentrated, and the target substance (1.50 g, 67%) was thus obtained as a light yellow solid.

後処理

  1. distillationThe solvent was distilled off under reduced pressure
  2. additiona small amount of ethanol and ethyl acetate were added to the residue
  3. customthe precipitate produced
  4. filtrationwas filtered off
  5. concentrationThe filtrate was concentrated
  6. customthe target substance (1.50 g, 67%) was thus obtained as a light yellow solid

出典と根拠

ORDレコード
ord-2661399e08f34854ab77fca9f20d2683
出典データセット
uspto-grants-2012_09
特許番号
US08268842B2

関連ノート

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