Sodium Carbonate → 2-Aminobenzimidazole

HRID 2166126Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2166126
ClCCOCC.Br.Br.N1CCC([NH:15][C:16]2[NH:20][C:19]3[CH:21]=[CH:22][CH:23]=[CH:24][C:18]=3[N:17]=2)CC1.C(=O)([O-])[O-].[Na+].[Na+].CN(C)C(=O)C>O>[NH:17]1[C:18]2[CH:24]=[CH:23][CH:22]=[CH:21][C:19]=2[N:20]=[C:16]1[NH2:15]

Komponenten

6

Edukt 4

HCID 10340Sodium CarbonateHCID 12341Ethane, 1-chloro-2-ethoxy-HCID 31374DimethylacetamideHCID 22036968N-(Piperidin-4-yl)-1H-benzo[d]imidazol-2-amine dihydrobromide

Produkt 1

HCID 136242-Aminobenzimidazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

A mixture of 32 parts of 1-chloro-2-ethoxyethane, 94.5parts of N-(4-piperidinyl)-1H-benzimidazol-2-amine dihydrobromide, 90 parts of sodium carbonate and 540 parts of N,N-dimethylacetamide was stirred overnight at 70° C. After cooling, the reaction mixture was poured into water. The product was extracted with dichloromethane. The extract was dried, filtered and evaporated. The residue was boiled in acetonitrile. After cooling, the precipitated product was filtered off and dried, yielding 42.4 parts (58.8%) of N-[1-(2-ethoxyethyl)-4-piperidinyl[-1H-benzimidazol-2-amine; mp. 212° C. (interm. 29).

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionThe product was extracted with dichloromethane
  3. customThe extract was dried
  4. filtrationfiltered
  5. customevaporated
  6. temperatureAfter cooling
  7. filtrationthe precipitated product was filtered off
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-a2dada330cdf4c488f3c7bb0c55e1fe3
Quelldatensatz
uspto-grants-1990_07
Patentnummer
US04943580

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