Reaktion #725764

ord-69f0d4ba43d44d7aa8d2768b08b45a09

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    Temperaturthe solution was heated
  2. 2
    Temperaturunder reflux for 6 hours
  3. 3
    workup.DISTILLATIONAt the end of this time, the solvent was distilled off
  4. 4
    Waschenthe residue was washed with water
  5. 5
    Sonstigedried in air
  6. 6
    SonstigeIt was then recrystallised from a mixture of benzene and hexane

Vorschrift

3.7 g (0.02 mole) of 4-chloro-3-methylthieno[2,3-d]pyrimidine, 4.6 g (0.02 mole) of 2-(2-chloro-6-methyl-4-propylphenoxy)ethylamine and 2 g (0.02 mole) of triethylamine were dissolved in 50 ml of benzene, and the solution was heated under reflux for 6 hours. At the end of this time, the solvent was distilled off and the residue was washed with water and dried in air. It was then recrystallised from a mixture of benzene and hexane, to give 4.5 g (yield 60%) of the desired Compound No. 19 in the form of colourless needles melting at 66°-68° C.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US04562193uspto-grants-1985_12