Reaktion #441979

ord-413d1d78ceff433fb65a7d6ff6b37fbd

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    SonstigeThe resulting reaction mixture
  2. 2
    Filtrationwas filtered
  3. 3
    workup.DISSOLUTIONThe crystalline solid was dissolved in 400 ml of 3 N hydrochloric acid
  4. 4
    Waschenthe aqueous acidic liquid was washed with ether
  5. 5
    Sonstigeprecipitated crystalline solid
  6. 6
    Sonstige6.8 g, m.p. 164°-166° C. (air dried)

Vorschrift

A mixture containing 9.6 g (0.04 mole) of 2-phenyl-4-chloroquinazoline, 6.4 g. (0.04 mole) of 1-(2-pyridyl) piperazine and 250 ml of isopropanol was refluxed for 4 hrs. The resulting reaction mixture was filtered after cooling to room temperature. The crystalline solid was dissolved in 400 ml of 3 N hydrochloric acid and the aqueous acidic liquid was washed with ether. The aqueous layer was adjusted to pH=7.5 which precipitated crystalline solid. This acidification and basification were repeated once. Yield of product was 6.8 g, m.p. 164°-166° C. (air dried).

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04377582uspto-grants-1983_03