Reaktion #1703300

ord-896bd2b3ce7445488231bf22f8956c9f

Lösungsmittel

Reaktionsbedingungen

Temperatur
100°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TemperaturThe mixture was then cooled to rt
  2. 2
    Einengenconcentrated
  3. 3
    SonstigeThe residue was purified by flash silica gel chromatography (0% to 5% MeOH/DCM)

Vorschrift

To a suspension of methyl 2-chloro-3-methyl-4-oxo-3,4-dihydroquinazoline-6-carboxylate (77.0 mg, 0.30 mmol) in isopropyl alcohol (5 mL) was added N,N-diisopropylethylamine (0.11 mL, 0.64 mmol) and 2-(4-chlorophenyl)ethanamine (0.11 mL, 0.76 mmol). The reaction mixture was heated to 100° C. and stirred for 1 h. The mixture was then cooled to rt and concentrated. The residue was purified by flash silica gel chromatography (0% to 5% MeOH/DCM) to afford methyl 2-{[2-(4-chlorophenyl)ethyl]amino}-3-methyl-4-oxo-3,4-dihydroquinazoline-6-carboxylate (106 mg, 94%). LC-MS: (FA) ES+ 372.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08765773B2uspto-grants-2014_07