Toluene → HCID 135984689, Verbindung

HRID 249778Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 249778
[CH3:1][C:2]1[N:6]=[C:5]([C:7]2[NH:11][CH:10]=[N:9][C:8]=2[NH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[NH:4][N:3]=1.[C:18](Cl)(Cl)=[O:19].C1(C)C=CC=CC=1>C1COCC1>[CH3:1][C:2]1[N:6]=[C:5]2[N:4]([C:18](=[O:19])[N:12]([CH2:13][CH2:14][CH2:15][CH2:16][CH3:17])[C:8]3[N:9]=[CH:10][NH:11][C:7]=32)[N:3]=1

Komponenten

5

Edukt 3

HCID 1140TolueneHCID 6371PhosgeneHCID 178446281HCID 178446281, Verbindung

Produkt 1

HCID 135984689HCID 135984689, VerbindungAusbeute 50 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of 5-(3-methyl-1H-1,2,4-triazol-5-yl)-N-pentyl-1H-imidazol-4-amine (45 mg, 0.19 mmol) in THF (10 mL) at 0° C. was added phosgene in toluene (0.3 mL, 1.0 mmol). The reaction mixture was slowly warmed to room temperature while stirring. The reaction mixture was concentrated under reduced pressure, and the residue was purified by preparative LCMS (method A) to provide the desired product (25 mg, 50% yield) as a white powder. LCMS calculated for C12H17N6O (M+H): 261.1. found: 261.1.

Aufarbeitung

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. customthe residue was purified by preparative LCMS (method A)

Quellen und Nachweise

ORD-Eintrag
ord-391e741a0cfa42b690a3931b4e111156
Quelldatensatz
uspto-grants-2011_01
Patentnummer
US07863285B2

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