Hydrochloric Acid → HCID 178515980, Verbindung

HRID 1176654Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1176654
C([N:20]1[CH:24]=[C:23]([C:25]2[CH:26]=[C:27]([OH:31])[CH:28]=[CH:29][CH:30]=2)[N:22]=[CH:21]1)(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1.CO.Cl.C(=O)([O-])O.[Na+]>C(Cl)(Cl)Cl>[NH:20]1[CH:24]=[C:23]([C:25]2[CH:26]=[C:27]([OH:31])[CH:28]=[CH:29][CH:30]=2)[N:22]=[CH:21]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 887MethanolHCID 516892Sodium BicarbonateHCID 684993453-(1-trityl-1H-imidazol-4-yl)phenol

Produkt 1

HCID 178515980HCID 178515980, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Versuchsvorschrift

A solution of 0.170 g of 3-(1-trityl-1H-imidazol-4-yl)phenol, 4.5 ml of methanol, 1.5 ml of chloroform and 1.5 ml of 2N HCl is stirred at 55° C. for 2 hours. After cooling, the reaction mixture is admixed with 35 ml of aqueous saturated sodium hydrogencarbonate solution and extracted twice with 75 ml of dichloromethane. The combined organic phases are washed with 35 ml of brine, dried over sodium sulphate and concentrated by evaporation. The title compound is obtained as a white solid from the residue by means of flash chromatography (SiO2 60F). Rf=0.14 (200:10:1 dichloromethane-methanol-conc. ammonia); Rt=2.08.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted twice with 75 ml of dichloromethane
  3. washThe combined organic phases are washed with 35 ml of brine
  4. dry with materialdried over sodium sulphate
  5. concentrationconcentrated by evaporation

Quellen und Nachweise

ORD-Eintrag
ord-4b1b703ae34d4c3985c93b90c2cb323c
Quelldatensatz
uspto-grants-2010_11
Patentnummer
US07842688B2

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