Potassium Carbonate → 1-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine

HRID 1493591

Reaktionsgleichung

Reaktionsgleichung von HRID 1493591
Cl.Cl.[CH3:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:7][CH:6]=1.Cl[C:18]1[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][N:19]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C.O>[CH3:3][O:4][C:5]1[CH:6]=[CH:7][C:8]([N:11]2[CH2:16][CH2:15][N:14]([C:18]3[CH:23]=[CH:22][C:21]([N+:24]([O-:26])=[O:25])=[CH:20][N:19]=3)[CH2:13][CH2:12]2)=[CH:9][CH:10]=1

Komponenten

6

Edukt 3

HCID 11430Potassium CarbonateHCID 783082-Chloro-5-nitropyridineHCID 27237001-(4-Methoxyphenyl)-piperazine, dihydrochloride

Produkt 1

HCID 37426761-(4-Methoxyphenyl)-4-(5-nitro-2-pyridinyl)piperazine

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A mixture of 1-(4-methoxyphenyl)piperazine dihydrochloride (5.30 g, 20 mmole), 2-chloro-5-nitropyridine (3.2 g, 20 mmole) and potassium carbonate (4.14 g, 30 mmole) in DMF (20 ml) was heated at 120° for 66 hours. The reaction mixture was cooled, diluted with water and the resulting precipitate collected by filtration. To this solid was added methanol (200 ml) and the mixture was heated under reflux for 0.17 hour. After cooling, the solid was collected by filtration and dried to yield the desired product, m.p. 165°-6° (4.0 g, 64%), which was used without further purification.

Aufarbeitung

  1. temperaturewas heated at 120° for 66 hours
  2. temperatureThe reaction mixture was cooled
  3. filtrationthe resulting precipitate collected by filtration
  4. additionTo this solid was added methanol (200 ml)
  5. temperaturethe mixture was heated
  6. temperatureunder reflux for 0.17 hour
  7. temperatureAfter cooling
  8. filtrationthe solid was collected by filtration
  9. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7c22ef8e681e4f7a8c12840adfc4c4bf
Quelldatensatz
uspto-grants-1991_06
Patentnummer
US05023258

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