Sodium hydride → HCID 57415861, Verbindung

HRID 2112612

Reaktionsgleichung

Reaktionsgleichung von HRID 2112612
[H-].[Na+].[CH3:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[C:9]#[N:10].[Cl-:11].[NH4+:12]>CO>[ClH:11].[CH3:3][N:4]1[CH:8]=[CH:7][N:6]=[C:5]1[C:9]([NH2:12])=[NH:10]

Komponenten

5

Edukt 3

HCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 109534431-Methyl-1H-imidazole-2-carbonitrile

Produkt 1

HCID 57415861HCID 57415861, VerbindungAusbeute 90,6 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To 10 mL of methyl alcohol in a sealed tube is added sodium hydride (440 mg, 11 mmol) with stirring. 1-Methyl-2-imidazole carbonitrile (1.18 g, 11 mmol) is added. The mixture is stirred at room temperature for 20 h, and ammonium chloride (588 mg, 11 mmol) is added. The bottle is then sealed and stirred at 80° C. for 8 h, and cooled to room temperature. The mixture is filtered, and the filtrate is concentrated. The residue is treated with 1% methyl alcohol in diethyl ether, and the precipitates are collected by filtration and dried to give 1-methyl-2-imidazole carboxamidine hydrochloride as a gray solid (1.6 g). MS: m/z 125.2 (M+H).

Aufarbeitung

  1. stirringThe mixture is stirred at room temperature for 20 h
  2. customThe bottle is then sealed
  3. stirringstirred at 80° C. for 8 h
  4. filtrationThe mixture is filtered
  5. concentrationthe filtrate is concentrated
  6. additionThe residue is treated with 1% methyl alcohol in diethyl ether
  7. filtrationthe precipitates are collected by filtration
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-7227f7d9235f4cfbb37c28f3ca1cff09
Quelldatensatz
uspto-grants-2009_04
Patentnummer
US07524849B2

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