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

HRID 326484

Reaktionsgleichung

Reaktionsgleichung von HRID 326484
[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, refilling when necessary. The mixture is filtered through celite, washed with ethanol, chloroform, ethanol and water. The organic solvents are removed with heat 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
  4. temperaturewith heat
  5. customThe remaining material is partitioned between methylene chloride (3×250 ml) and sodium bicarbonate
  6. dry with materialdried over potassium carbonate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customto give an oil which

Quellen und Nachweise

ORD-Eintrag
ord-55e9d79048d24531bc55fa44cf591181
Quelldatensatz
uspto-grants-1993_12
Patentnummer
US05268477

Verknüpfte Notizen

Wird geladen…