Reaktion #64276
ord-d3d3bb326fba4875ab2dbbc113d0b222
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1Sonstigeby bubbling the gas through dry methanol for several minutes
- 2workup.DISSOLUTIONhad completely dissolved (about 13 mL)
- 3workup.WAITAfter the resulting mixture had stood at about 25° C. for several minutes
- 4Sonstigea precipitate formed
- 5TemperaturThe mixture was cooled in an ice bath for thirty minutes
- 6Filtrationthe 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.