Hydrochloric Acid → 1-methyl-2-(piperazin-1-yl)-1H-benzo[d]imidazole

HRID 2415863Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2415863
Cl[C:2]1[N:6]([CH3:7])[C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=1.[NH:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1.Cl>O>[CH3:7][N:6]1[C:5]2[CH:8]=[CH:9][CH:10]=[CH:11][C:4]=2[N:3]=[C:2]1[N:12]1[CH2:17][CH2:16][NH:15][CH2:14][CH2:13]1

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 4837PiperazineHCID 6630802-chloro-1-methyl-1H-1,3-benzodiazole

Produkt 1

HCID 6675511-methyl-2-(piperazin-1-yl)-1H-benzo[d]imidazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
150 °C

Versuchsvorschrift

A mixture of 1 g (6.02 mmol) of 2-chloro-1-methyl-benzimidazole and 2.58 g (30 mmol) of piperazine is heated to 150° C. without a solvent. The cooled melt is combined successively with water and dilute hydrochloric acid and extracted with dichloromethane. Then the aqueous phase is made alkaline with dilute sodium hydroxide solution and extracted with dichloromethane. The organic phase is dried over sodium sulphate and concentrated by evaporation. The product is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia=5:1:0.1).

Aufarbeitung

  1. extractionextracted with dichloromethane
  2. extractionextracted with dichloromethane
  3. dry with materialThe organic phase is dried over sodium sulphate
  4. concentrationconcentrated by evaporation
  5. customThe product is purified by column chromatography on silica gel (eluant: dichloromethane/ethanol/ammonia=5:1:0.1)

Quellen und Nachweise

ORD-Eintrag
ord-2fa0de9281d94d13a7aafd0340a3f084
Quelldatensatz
uspto-grants-2004_11
Patentnummer
US06821967B2

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