Urea → HCID 67151381, Verbindung

HRID 2064238Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2064238
N([O-])=O.[Na+].[N:5]1([C:11]([C:13]2[N:18]=[CH:17][C:16](N)=[CH:15][CH:14]=2)=[O:12])[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]1.NC(N)=O.[I-:24].[Na+]>Cl>[I:24][C:16]1[CH:15]=[CH:14][C:13]([C:11]([N:5]2[CH2:10][CH2:9][CH2:8][CH2:7][CH2:6]2)=[O:12])=[N:18][CH:17]=1

Komponenten

6

Edukt 4

HCID 1176UreaHCID 5238Sodium IodideHCID 23668193Sodium NitriteHCID 671512216-[(Piperidin-1-yl)carbonyl]pyridin-3-amine

Produkt 1

HCID 67151381HCID 67151381, VerbindungAusbeute 23 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

A solution of sodium nitrite (69 g) in concentrated hydrochloric acid (1.5 L) was added to crude 6-(piperidin-1-ylcarbonyl)pyridin-3-amine at 0 C, and the mixture was stirred for 10 minutes. Urea (20 g) was added, and the mixture was stirred for 15 minutes. Sodium iodide (150 g) was added, and the product was separated by filtration and recrystallized from ethanol to give 5-iodo-2-(piperidin-1-ylcarbonyl)pyridine (yield 23% calculated for methyl 5-nitropyridine-2-carboxylate, 71 g).

Aufarbeitung

  1. stirringthe mixture was stirred for 15 minutes
  2. customthe product was separated by filtration
  3. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-5d7cfa3f9f034f9d8d8f3bf21c39f1a2
Quelldatensatz
uspto-grants-2012_10
Patentnummer
US08288405B2

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