Réaction #528484

ord-75174040face4dd6bb12d3b6d16d90a9

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    Températureunder reflux for 2 hours
  2. 2
    AutreAfter neutralization and evaporation
  3. 3
    Autrein vacuo, purification of the residue over silica gel
  4. 4
    Autrewith methylene chloride/propanol (8:2) and recrystallization from ethanol

Mode opératoire

4.0 G. of 5'-[(2,4-diamino-5-pyrimidinyl)methyl]3'-dimethylamino-2'-methoxy-N-methylacetanilide (prepared as described in the first paragraph of Example 2) and 100 ml. of 1-N hydrochloric acid were boiled under reflux for 2 hours. After neutralization and evaporation in vacuo, purification of the residue over silica gel with methylene chloride/propanol (8:2) and recrystallization from ethanol, there was obtained 2,4-diamino-5-[3-dimethylamino-4-methoxy-5-(methylamino)benzyl]pyrimidine, having a melting point of 183° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04039543uspto-grants-1977_08