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Ammonium Hydroxide → 8-benzyloxy-2-(ethoxymethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-4-amine

HRID 540946
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 540946
C1C=C(Cl)C=C(C(OO)=O)C=1.[CH2:12]([O:19][C:20]1[CH:29]=[CH:28][C:27]2[N:26]=[CH:25][C:24]3[N:30]=[C:31]([CH2:36][O:37][CH2:38][CH3:39])[N:32]([CH2:33][CH2:34][CH3:35])[C:23]=3[C:22]=2[CH:21]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.ClC(Cl)(Cl)C([N:44]=C=O)=O.[OH-].[NH4+]>ClCCl>[CH2:12]([O:19][C:20]1[CH:29]=[CH:28][C:27]2[N:26]=[C:25]([NH2:44])[C:24]3[N:30]=[C:31]([CH2:36][O:37][CH2:38][CH3:39])[N:32]([CH2:33][CH2:34][CH3:35])[C:23]=3[C:22]=2[CH:21]=1)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 14923Ammonium HydroxideHCID 70297m-Chloroperbenzoic acidHCID 76400Trichloroacetyl isocyanateHCID 670511278-benzyloxy-2-ethoxymethyl-1-propyl-1H-imidazo[4,5-c]quinoline

Produkt 1

HCID 575453188-benzyloxy-2-(ethoxymethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-4-amine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

mCPBA (60% pure, 27.5 g, 95.9 mmol) was added in small portions over a period of 20 minutes to 8-benzyloxy-2-(ethoxymethyl)-1-propyl-1H-imidazo[4,5-c]quinoline (30.0 g, 79.9 mmol, prepared in Parts A through H of Example 2) in dichloromethane (400 mL). After the reaction was stirred for two hours, it was washed with 1% aqueous sodium carbonate (3×100 mL). The combined aqueous washings were extracted with chloroform (200 mL), and the combined organic fractions were dried over magnesium sulfate and filtered. Trichloroacetyl isocyanate (18.0 g, 95.9 mmol) was added dropwise to the filtrate, and then the reaction was stirred overnight at ambient temperature. Concentrated ammonium hydroxide (100 mL) was slowly added, and the mixture was stirred at ambient temperature for 30 minutes. The organic layer was separated and washed with 1% aqueous sodium carbonate (2×100 mL). The combined aqueous fractions were extracted with chloroform (3×75 mL). The organic fractions were combined, dried over magnesium sulfate, filtered, and concentrated under reduced pressure to yield a dark semi-solid. The crude product was purified on silica gel (1 kg, eluting sequentially with 2% methanol in chloroform and 5% methanol in chloroform) to provide 22 g of 8-benzyloxy-2-(ethoxymethyl)-1-propyl-1H-imidazo[4,5-c]quinolin-4-amine as an off-white solid.

Aufarbeitung

  1. washit was washed with 1% aqueous sodium carbonate (3×100 mL)
  2. extractionThe combined aqueous washings were extracted with chloroform (200 mL)
  3. dry with materialthe combined organic fractions were dried over magnesium sulfate
  4. filtrationfiltered
  5. stirringthe reaction was stirred overnight at ambient temperature
  6. stirringthe mixture was stirred at ambient temperature for 30 minutes
  7. customThe organic layer was separated
  8. washwashed with 1% aqueous sodium carbonate (2×100 mL)
  9. extractionThe combined aqueous fractions were extracted with chloroform (3×75 mL)
  10. dry with materialdried over magnesium sulfate
  11. filtrationfiltered
  12. concentrationconcentrated under reduced pressure
  13. customto yield a dark semi-solid
  14. customThe crude product was purified on silica gel (1 kg
  15. washeluting sequentially with 2% methanol in chloroform and 5% methanol in chloroform)

Quellen und Nachweise

ORD-Eintrag
ord-c1c8baaab91e493293c5443dd27c80ad
Quelldatensatz
uspto-grants-2014_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08871782B2

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