Reaktion #1447

ord-8d43c74a9d90473996cdace2ba79d6f8

Reaktionsgleichung

COc1ccccc1-c1ccc(C(=O)N2CCc3nc(C)[nH]c3-c3ccccc32)cc1
6-[(2'-Methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine
CCOC(C)=O.Cl
hydrochloric acid ethyl acetate
COc1ccccc1-c1ccc(C(=O)N2CCc3nc(C)[nH]c3-c3ccccc32)cc1.Cl
6-[(2'-methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine hydrochloride

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturcooled on an ice bath to effect crystal formation
  2. 2
    Filtrationthe thus formed crystals were collected by filtration
  3. 3
    Waschenwashed with a small volume of ethyl alcohol

Vorschrift

6-[(2'-Methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine was dissolved in 4.8 ml of ethyl alcohol, the solution was mixed with 0.44 ml of 4N hydrochloric acid-ethyl acetate and cooled on an ice bath to effect crystal formation, and then the thus formed crystals were collected by filtration and washed with a small volume of ethyl alcohol to obtain 260 mg of 6-[(2'-methoxy-4-biphenylyl)carbonyl]-2-methyl-1,4,5,6-tetrahydroimidazo[4,5-d][1]benzazepine hydrochloride (Example 33(2)).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05723606uspto-grants-1998_03