Diethyl Ether → HCID 10126861, Verbindung

HRID 11341

Reaktionsgleichung

Reaktionsgleichung von HRID 11341
[C:1]1([N:7]=[C:8]=[O:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH2:10][CH2:11][CH2:12][CH2:13][CH2:14][N:15]1[C:23]2[C:22]([CH3:24])=[C:21]([CH3:25])[N:20]=[C:19]([NH2:26])[C:18]=2[N:17]=[C:16]1[CH2:27][CH2:28][CH2:29][CH3:30].C(OCC)C>ClCCl>[NH2:26][C:19]1[C:18]2[N:17]=[C:16]([CH2:27][CH2:28][CH2:29][CH3:30])[N:15]([CH2:14][CH2:13][CH2:12][CH2:11][NH:10][C:8]([NH:7][C:1]3[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=3)=[O:9])[C:23]=2[C:22]([CH3:24])=[C:21]([CH3:25])[N:20]=1

Komponenten

5

Edukt 3

HCID 3283Diethyl EtherHCID 7672Phenyl isocyanateHCID 120210831-(4-aminobutyl)-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine

Produkt 1

HCID 10126861HCID 10126861, VerbindungAusbeute 90,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

Phenylisocyanate (0.056 mL, 0.5 mmol) was added to a chilled solution of of 1-(4-aminobutyl)-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-4-amine (150 mg, 0.5 mmol) in dichloromethane (150 mL). The ice bath was removed. A white precipitate formed after 5 minutes. The reaction mixture was allowed to stir for 30 minutes and then it was concentrated under reduced pressure to provide an off-white crystalline solid. This material was isolated by filtration using a small amount of diethyl ether to transfer the material to the filter and then dried in an Abderhalden drying apparatus to provide 185 mg of N-[4-(4-amino-2-butyl-6,7-dimethyl-1H-imidazo[4,5-c]pyridin-1-yl)butyl]-N′-phenylurea, m.p. 195.8–196.8° C.

Aufarbeitung

  1. customThe ice bath was removed
  2. customA white precipitate formed after 5 minutes
  3. concentrationit was concentrated under reduced pressure
  4. customto provide an off-white crystalline solid
  5. customThis material was isolated by filtration
  6. filtrationfilter
  7. customdried in an Abderhalden
  8. customdrying apparatus

Quellen und Nachweise

ORD-Eintrag
ord-4a854fb3441e4f0bb5ab3b1ac5e53424
Quelldatensatz
uspto-grants-2006_08
Patentnummer
US07098221B2

Verknüpfte Notizen

Wird geladen…