Reaktion #672275

ord-f71b336ecbd14ceb93b756c708a78a53

Lösungsmittel

Reaktionsbedingungen

Temperatur
55°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeVolatiles were evaporated
  2. 2
    Sonstigethe residue was partitioned between methylene chloride and saturated solution of ammonium hydroxide
  3. 3
    TrocknenThe organic phase was dried over anhydrous sodium sulfate
  4. 4
    Einengenconcentrated in vacuo

Vorschrift

A solution of 2,4,6-trichloroquinazoline (0.186 g, 0.80 mmol) in ethanol (20 ml) was heated to 55° C. and piperonylamine (0.145 g, 0.96 mmol) was added. The resulting mixture was stirred at 55° C. over night. Volatiles were evaporated and the residue was partitioned between methylene chloride and saturated solution of ammonium hydroxide. The organic phase was dried over anhydrous sodium sulfate and concentrated in vacuo to yield 0.268 g (96% yield) of the title compound as a white solid. 1H NMR (300 MHz, DMSO) δ 4.59-4.63 (d, 2H), 5.98 (s, 2H), 6.86 (s, 2H), 6.96 (s, 1H), 7.62-7.66 (d, 1H), 7.79-7.84 (d, 1H), 8.46 (s, 1H), 9.24-9.28 (t,1H).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US06930113B2uspto-grants-2005_08