Hydrochloric Acid → 2-(Piperazin-1-yl)pyridin-3-amine

HRID 982526

Reaktionsgleichung

Reaktionsgleichung von HRID 982526
[N:1]1([C:7]2[C:12]([N+:13]([O-])=O)=[CH:11][CH:10]=[CH:9][N:8]=2)[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.Cl>C(O)C>[NH2:13][C:12]1[C:7]([N:1]2[CH2:2][CH2:3][NH:4][CH2:5][CH2:6]2)=[N:8][CH:9]=[CH:10][CH:11]=1

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 37788341-(3-Nitropyridin-2-yl)piperazine

Produkt 1

HCID 103973582-(Piperazin-1-yl)pyridin-3-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

2-(1-Piperazinyl)-3-nitropyridine (24.50 g), ethanol (445 ml) and hydrochloric acid (1.2N, 44 ml) are combined and hydrogenated overnight at 40 psi initial pressure in a Parr Bomb, refilling when necessary. The mixture is filtered through celite, washed with ethanol, chloroform, ethanol and water. The organic solvents are removed with head and reduced pressure. The remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate. The organic layers are combined, dried over potassium carbonate, filtered and concentrated under reduced pressure to give an oil which slowly solidified upon standing to give 3-amino-2-(1-piperazinyl)pyridine.

Aufarbeitung

  1. filtrationThe mixture is filtered through celite
  2. washwashed with ethanol, chloroform, ethanol and water
  3. customThe organic solvents are removed with head and reduced pressure
  4. customThe remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate
  5. dry with materialdried over potassium carbonate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customto give an oil which

Quellen und Nachweise

ORD-Eintrag
ord-d26c1200618a4cfeb5e8d205a7108f65
Quelldatensatz
uspto-grants-1991_02
Patentnummer
US04996318

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