Hydrochloric Acid → HCID 20078040, Verbindung

HRID 1654478Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1654478
Cl[C:2]1[N:6]([CH:7]([CH3:9])[CH3:8])[C:5]2[CH:10]=[CH:11][C:12]([Cl:14])=[CH:13][C:4]=2[N:3]=1.[CH3:15][N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1.Cl>>[Cl:14][C:12]1[CH:11]=[CH:10][C:5]2[N:6]([CH:7]([CH3:9])[CH3:8])[C:2]([N:19]3[CH2:20][CH2:21][N:16]([CH3:15])[CH2:17][CH2:18]3)=[N:3][C:4]=2[CH:13]=1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 531671-MethylpiperazineHCID 20078039HCID 20078039, Verbindung

Produkt 1

HCID 20078040HCID 20078040, VerbindungAusbeute 46,9 %

Reaktionsbedingungen

Temperatur
140 °C

Versuchsvorschrift

A mixture of 2,5-dichloro-1-isopropylbenzimidazole (7 g) and N-methylpiperazine (10 g) was stirred at 140° C. for 3.5 hours. After cooling, 2N hydrochloric acid was added to the mixture and the mixture was washed with ethyl acetate. The 2N hydrochloric acid layer was made basic with an aqueous 2N sodiumhydroxide solution and extracted with ethyl acetate. The ethyl acetate layer was washed with a saturated sodium chloride solution and dried over anhydrous magnesium sulfate and then the solvent was distilled off under reduced pressure to give 5-chloro-1-isopropyl-2-(4-methyl-1-piperazinyl)benzimidazole (4.2 g). A part of the obtained product was recrystallized from acetonitrile, which showed the following physical properties:

Aufarbeitung

  1. temperatureAfter cooling
  2. washthe mixture was washed with ethyl acetate
  3. extractionextracted with ethyl acetate
  4. washThe ethyl acetate layer was washed with a saturated sodium chloride solution
  5. dry with materialdried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-bbbca3b7e749445bbd1b5ce1dea5c822
Quelldatensatz
uspto-grants-1995_04
Patentnummer
US05407936

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