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Cyanogen Bromide → HCID 86626274, Verbindung

HRID 1097549
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1097549
[Cl:1][C:2]1[C:11]([NH2:12])=[C:10]([NH:13][CH2:14][CH:15]([CH3:17])[CH3:16])[C:9]2[C:4](=[CH:5][CH:6]=[CH:7][CH:8]=2)[N:3]=1.[N:18]#[C:19][Br:20]>C(O)C>[BrH:20].[Cl:1][C:2]1[C:11]2[N:12]=[C:19]([NH2:18])[N:13]([CH2:14][CH:15]([CH3:17])[CH3:16])[C:10]=2[C:9]2[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=2[N:3]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 10476Cyanogen BromideHCID 117470392-Chloro-N4-(2-methylpropyl)-3,4-quinolinediamine

Produkt 1

HCID 86626274HCID 86626274, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Versuchsvorschrift

A solution of 2-chloro-N4-(2-methylpropyl)-3,4-quinolinediamine (André et al, U.S. Pat. No. 4,988,815, Example 6, 8.92 g, 35.7 mmol) in ethanol (50 mL) was stirred at 100° C.; cyanogen bromide (5.67 g, 53.5 mmol) was added in one portion. The red solution was stirred overnight, washed three times with water, and washed once with brine. A precipitate formed in the aqueous washings and was isolated by filtration. The organic fraction was dried over magnesium sulfate, filtered through a layer of CELITE filer agent, concentrated under reduced pressure, further dried under high vacuum, and combined with the isolated precipitate to provide 9.81 g of 4-chloro-1-(2-methylpropyl)-1H-imidazo[4,5-c]quinoline-2-amine hydrobromide as a dark red solid.

Aufarbeitung

  1. washwashed three times with water
  2. washwashed once with brine
  3. customA precipitate formed in the aqueous washings
  4. customwas isolated by filtration
  5. dry with materialThe organic fraction was dried over magnesium sulfate
  6. filtrationfiltered through a layer of CELITE filer agent
  7. concentrationconcentrated under reduced pressure
  8. customfurther dried under high vacuum

Quellen und Nachweise

ORD-Eintrag
ord-a198fe4280b4467b9588fb7e93c36643
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08143270B2

Notizen zur Reaktion

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