Hydrogen Bromide → HCID 19353953, Verbindung

HRID 741730Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 741730
[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([O:22]C)[CH:17]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br>C(O)(=O)C>[C:1]1([N:7]2[C:11]3[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=3[N:9]=[C:8]2[C:16]2[CH:21]=[CH:20][CH:19]=[C:18]([OH:22])[CH:17]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

Komponenten

4

Edukt 2

HCID 260Hydrogen BromideHCID 193539742-(3-Methoxyphenyl)-1-phenyl-1H-benzimidazole

Produkt 1

HCID 19353953HCID 19353953, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Versuchsvorschrift

A solution of 1-phenyl-2-(3-methoxyphenyl)benzimidazole (0.20 g, 0.67 mmol) and hydrobromic acid (4 ml) and acetic acid (4 ml) was refluxed for 48 hours. The reaction mixture was cooled and extracted with diethyl ether (5×150 ml) at pH 3-5. The organic fractions were discarded. The aqueous phase was alkalinized to pH 8-9 and extracted with ethyl acetate (5×150 ml). The organic layers were combined, washed with a saturated sodium chloride solution, dried over magnesium sulfate, filtered, and the solvents were removed in vacuo to yield a white solid. The solid was triturated with an ethyl acetate/diethyl ether mixture.

Aufarbeitung

  1. temperatureThe reaction mixture was cooled
  2. extractionextracted with diethyl ether (5×150 ml) at pH 3-5
  3. extractionextracted with ethyl acetate (5×150 ml)
  4. washwashed with a saturated sodium chloride solution
  5. dry with materialdried over magnesium sulfate
  6. filtrationfiltered
  7. customthe solvents were removed in vacuo
  8. customto yield a white solid
  9. customThe solid was triturated with an ethyl acetate/diethyl ether mixture

Quellen und Nachweise

ORD-Eintrag
ord-c28f541c939c45ff9039bc35ecd859cf
Quelldatensatz
uspto-grants-1996_09
Patentnummer
US05552426

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