Potassium Carbonate → HCID 22724164, Verbindung

HRID 2231003Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2231003
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:11][C:12]1[CH:13]=[C:14]([NH:18][C:19]([C:21]2[CH:30]=[CH:29][C:28]3[C:23](=[CH:24][CH:25]=[CH:26][CH:27]=3)[CH:22]=2)=[O:20])[CH:15]=[CH:16][CH:17]=1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[CH:22]1[C:23]2[C:28](=[CH:27][CH:26]=[CH:25][CH:24]=2)[CH:29]=[CH:30][C:21]=1[C:19]([NH:18][C:14]1[CH:13]=[C:12]([NH:11][C:2]2[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=2)[CH:17]=[CH:16][CH:15]=1)=[O:20]

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 796132-Chloro-3-nitropyridineHCID 16774264HCID 16774264, Verbindung

Produkt 1

HCID 22724164HCID 22724164, VerbindungAusbeute 50,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

A mixture of 2-chloro-3-nitropyridine (0.87 g), N-(3-aminophenyl)-2-naphthalenecarboxamide (1.31 g) and potassium carbonate (1.0 g) in 1,4-dioxane (20 ml) was stirred under reflux for 20 hours. After cooling, insoluble materials were removed by filtration and the filtrate was concentrated. The resultant solid was collected and washed with isopropyl ether to give 2-[3-(2-naphthoylamino)phenylamino]-3-nitropyridine (961 mg) as an orange solid.

Aufarbeitung

  1. temperatureunder reflux for 20 hours
  2. temperatureAfter cooling
  3. custominsoluble materials were removed by filtration
  4. concentrationthe filtrate was concentrated
  5. customThe resultant solid was collected
  6. washwashed with isopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-bf8772787cee47e883202892f2391193
Quelldatensatz
uspto-grants-2002_07
Patentnummer
US06426345B1

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