Ammonia → HCID 178508170, Verbindung

HRID 388616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 388616
[Si]([O:8][CH2:9][CH2:10][CH2:11][CH2:12][N:13]1[C:25]2[C:24]3[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=3[N:18]=[C:17](Cl)[C:16]=2[N:15]=[C:14]1[OH:27])(C(C)(C)C)(C)C.[NH3:28]>CO>[NH2:28][C:17]1[C:16]2[N:15]=[C:14]([OH:27])[N:13]([CH2:12][CH2:11][CH2:10][CH2:9][OH:8])[C:25]=2[C:24]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[N:18]=1

Komponenten

4

Edukt 2

HCID 222AmmoniaHCID 178455216HCID 178455216, Verbindung

Produkt 1

HCID 178508170HCID 178508170, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

1-[4-(tert-Butyldimethylsilanyloxy)butyl]-4-chloro-1H-imidazo[4,5-c]quinolin-2-ol (5.0 g, 12 mmol) and ammonia (200 mL of a 7 N solution in methanol) were added to a high-pressure vessel, which was sealed and heated in an oven at 150° C. for five days, allowed to cool, and concentrated under reduced pressure. The crude product was triturated with hexane for 15 minutes, and the resulting solid was isolated by filtration, washed with hexane (500 mL), and dried under vacuum to provide 3.53 g of 4-amino-1-(4-hydroxybutyl)-1H-imidazo[4,5-c]quinolin-2-ol as a light gray solid.

Aufarbeitung

  1. customwhich was sealed
  2. temperatureto cool
  3. concentrationconcentrated under reduced pressure
  4. customThe crude product was triturated with hexane for 15 minutes
  5. customthe resulting solid was isolated by filtration
  6. washwashed with hexane (500 mL)
  7. customdried under vacuum

Quellen und Nachweise

ORD-Eintrag
ord-0794f5e19dc34465b4c1fd33f406e10c
Quelldatensatz
uspto-grants-2013_02
Patentnummer
US08377957B2

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