Reaktion #64276

ord-d3d3bb326fba4875ab2dbbc113d0b222

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Sonstigeby bubbling the gas through dry methanol for several minutes
  2. 2
    workup.DISSOLUTIONhad completely dissolved (about 13 mL)
  3. 3
    workup.WAITAfter the resulting mixture had stood at about 25° C. for several minutes
  4. 4
    Sonstigea precipitate formed
  5. 5
    TemperaturThe mixture was cooled in an ice bath for thirty minutes
  6. 6
    Filtrationthe precipitated solid collected by filtration

Vorschrift

A solution of hydrogen chloride in methanol was prepared by bubbling the gas through dry methanol for several minutes. 1-(4-Amino-6,7-dimethoxy-2-quinazolinyl)-4-(tetrahydro-2-furoyl)piperazine (1.2 g, 3.1 mmol) was placed in an Erlenmeyer flask, together with a magnetic stirring bar, and the methanolic solution of hydrogen chloride was added until the solid had completely dissolved (about 13 mL). After the resulting mixture had stood at about 25° C. for several minutes, a precipitate formed. The mixture was cooled in an ice bath for thirty minutes and the precipitated solid collected by filtration to yield 1.1 g (2.41 mmol, 77.8%) of 1-(4-amino-6,7-dimethoxy-2-quinazolinyl)-4-(tetrahydro-2-furoyl)piperazine monohydrochloride methanolate.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US05412095uspto-grants-1995_05