Hydrochloric Acid → 3-Aminopicolinic acid

HRID 2386974

반응식

HRID 2386974 반응식
[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

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 516892Sodium BicarbonateHCID 183766123-Nitropyridine-2-carboxylic acidHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 738363-Aminopicolinic acid

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-2661399e08f34854ab77fca9f20d2683
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08268842B2

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