Guanidine → HCID 178510034, Verbindung

HRID 25053

Reaktionsgleichung

Reaktionsgleichung von HRID 25053
[OH-].[Na+].[NH2:3][C:4]([NH2:6])=[NH:5].Cl[C:8]1[N:13]=[C:12]([CH2:14][C:15]2[C:20]([Cl:21])=[CH:19][CH:18]=[CH:17][C:16]=2[Cl:22])[N:11]=[C:10]([NH:23][C:24]2[CH:31]=[CH:30][C:27]([C:28]#[N:29])=[CH:26][CH:25]=2)[N:9]=1>O1CCOCC1>[C:28]([C:27]1[CH:30]=[CH:31][C:24]([NH:23][C:10]2[N:11]=[C:12]([CH2:14][C:15]3[C:20]([Cl:21])=[CH:19][CH:18]=[CH:17][C:16]=3[Cl:22])[N:13]=[C:8]([NH:5][C:4]([NH2:6])=[NH:3])[N:9]=2)=[CH:25][CH:26]=1)#[N:29]

Komponenten

5

Edukt 3

HCID 3520GuanidineHCID 14798Sodium HydroxideHCID 4864234-[[4-Chloro-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]amino]benzonitrile

Produkt 1

HCID 178510034HCID 178510034, VerbindungAusbeute 64,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

NaOH (0.0128 mol), 1,4-dioxane (5 ml), and guanidine (0.0128 mol) were combined and stirred at RT for 5 minutes under argon. Then, intermediate (27) (0.00128 mol) was added and the reaction mixture was stirred at RT for 16 hours. The reaction mixture was quenched with H2O, and stirred. The resulting precipitate was filtered off and the residue was stirred in refluxing methanol, cooled, and filtered, yielding 0.34 g (64.3%) of N-[4-[(4-cyanophenyl)amino]-6-[(2,6-dichlorophenyl)methyl]-1,3,5-triazin-2-yl]-guanidine (compound 20).

Aufarbeitung

  1. stirringthe reaction mixture was stirred at RT for 16 hours
  2. customThe reaction mixture was quenched with H2O
  3. stirringstirred
  4. filtrationThe resulting precipitate was filtered off
  5. stirringthe residue was stirred
  6. temperaturein refluxing methanol
  7. temperaturecooled
  8. filtrationfiltered

Quellen und Nachweise

ORD-Eintrag
ord-46fa65e8e380434ab77bc22111932839
Quelldatensatz
uspto-grants-2005_02
Patentnummer
US06858609B2

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