StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

Hydrochloric Acid → 8-(2-aminoethoxy)-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinolin-4-amine

HRID 2203494
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 2203494
Cl.[NH2:2][C:3]1[C:12]2[N:13]=[C:14]([CH2:19][O:20][CH2:21][CH3:22])[N:15]([CH2:16][CH2:17][CH3:18])[C:11]=2[C:10]2[CH:9]=[C:8]([O:23][CH2:24][CH2:25][NH:26]C(=O)OC(C)(C)C)[CH:7]=[CH:6][C:5]=2[N:4]=1>C(O)C>[NH2:26][CH2:25][CH2:24][O:23][C:8]1[CH:7]=[CH:6][C:5]2[N:4]=[C:3]([NH2:2])[C:12]3[N:13]=[C:14]([CH2:19][O:20][CH2:21][CH3:22])[N:15]([CH2:16][CH2:17][CH3:18])[C:11]=3[C:10]=2[CH:9]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 68974513tert-butyl 2-[(4-amino-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinolin-8-yl)oxy]ethylcarbamate

Produkt 1

HCID 588336918-(2-aminoethoxy)-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinolin-4-amineAusbeute 85,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of hydrogen chloride (55 mL of 1.2 M) in ethanol was added to tert-butyl 2-[(4-amino-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinolin-8-yl)oxy]ethylcarbamate (3.98 g, 8.97 mmol), and the reaction was heated at reflux for one hour. The reaction mixture was allowed to cool to ambient temperature, and the solvent was removed under reduced pressure. The resulting yellow solid was dissolved in a small volume of water, and 10% aqueous sodium hydroxide was added to adjust to pH 13. The mixture was then extracted with dichloromethane (3×100 mL), and the combined extracts were washed sequentially with water and brine, dried over magnesium sulfate, and concentrated under reduced pressure. The resulting solid was recrystallized from acetonitrile to provide 2.63 g of 8-(2-aminoethoxy)-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinolin-4-amine as fine, peach-colored needles, mp 157-159° C.

Aufarbeitung

  1. temperaturethe reaction was heated
  2. temperatureat reflux for one hour
  3. customthe solvent was removed under reduced pressure
  4. dissolutionThe resulting yellow solid was dissolved in a small volume of water, and 10% aqueous sodium hydroxide
  5. additionwas added
  6. extractionThe mixture was then extracted with dichloromethane (3×100 mL)
  7. washthe combined extracts were washed sequentially with water and brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe resulting solid was recrystallized from acetonitrile

Quellen und Nachweise

ORD-Eintrag
ord-c6eaee18750c4d44beadfc2ffed4112c
Quelldatensatz
uspto-grants-2016_06
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09365567B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion