N,N-Dimethylethylenediamine → 2-[2-(dimethylamino)ethylamino]-4-nitro-1H-benzimidazole

HRID 1533780Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1533780
Cl[C:2]1[NH:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:4]=2[N:3]=1.[CH3:14][N:15]([CH3:19])[CH2:16][CH2:17][NH2:18].C(=O)(O)[O-].[Na+]>>[CH3:14][N:15]([CH3:19])[CH2:16][CH2:17][NH:18][C:2]1[NH:6][C:5]2[CH:7]=[CH:8][CH:9]=[C:10]([N+:11]([O-:13])=[O:12])[C:4]=2[N:3]=1

Komponenten

4

Reaktionsbedingungen

Temperatur
80 °C

Versuchsvorschrift

A mixture of 2-chloro-4-nitro-1H-benzimidazole (300 mg) and N,N-dimethylethylenediamine (2 ml) were stirred at 80° C. for 8 hours. The reaction mixture was poured into saturated sodium bicarbonate aqueous solution and extracted with a mixture of chloroform and methanol. The organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was washed with diisopropyl ether to give 2-[[2-(dimethylamino)ethyl]amino]-4-nitro-1H-benzimidazole (113 mg).

Aufarbeitung

  1. extractionextracted with a mixture of chloroform and methanol
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. washThe residue was washed with diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-e6179ebf95bd4aa2a97232e4d303c645
Quelldatensatz
uspto-grants-2001_03
Patentnummer
US06207693B1

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