Chloroform → 1H-Benzimidazol-6-amine,1,2-dimethyl-(9CI)

HRID 230851Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 230851
O.O.[Sn](Cl)Cl.[CH3:6][N:7]1[C:11]2[CH:12]=[C:13]([N+:16]([O-])=O)[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH3:19].C(Cl)(Cl)Cl.[OH-].[Na+]>Cl>[CH3:6][N:7]1[C:11]2[CH:12]=[C:13]([NH2:16])[CH:14]=[CH:15][C:10]=2[N:9]=[C:8]1[CH3:19]

Komponenten

6

Edukt 4

HCID 6212ChloroformHCID 14798Sodium HydroxideHCID 61436Stannous chloride dihydrateHCID 133278651,2-dimethyl-6-nitro-1H-benzo[d]imidazole

Produkt 1

HCID 122280631H-Benzimidazol-6-amine,1,2-dimethyl-(9CI)

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 313Hydrochloric AcidLösungsmittel

Versuchsvorschrift

To a stirred solution of tin (II) chloride dihydrate (4.7 g) in concentrated hydrochloric acid (15 ml) was added 1,2-dimethyl-6-nitro-1H-benzimidazole (1 g) (J. Chem. Soc.,1931, 1143-1153), and the mixture was stirred at room temperature for 6 h. The mixture was poured onto ice and chloroform, and basified to pH 10 by the addition of 10M sodium hydroxide solution. The mixture was extracted several times with chloroform and the combined organic extracts dried and concentrated in vacuo to give a brown solid. This was crystallised from ethanol to give the title compound.

Aufarbeitung

  1. extractionThe mixture was extracted several times with chloroform
  2. customthe combined organic extracts dried
  3. concentrationconcentrated in vacuo
  4. customto give a brown solid
  5. customThis was crystallised from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-15e3655b520144ca863276a4bcec9132
Quelldatensatz
uspto-grants-2009_07
Patentnummer
US07566786B2

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