Réaction #63647

ord-db1c7b5655734fdd82605a2897516b93

Conditions de réaction

Conditions détaillées
See reaction.notes.procedure_details.

Traitement

  1. 1
    TempératureThe reaction mixture was refluxed overnight
  2. 2
    Autredimethylformamide was evaporated under reduced pressure
  3. 3
    Extractionthe residue was extracted with methylene chloride (400 ml.)
  4. 4
    AutreThe methylene chloride extracts were collected
  5. 5
    Lavagewashed with water
  6. 6
    Autreevaporated
  7. 7
    Autrethe remaining residue was purified by HPLC
  8. 8
    Autreto give 1.3 g

Mode opératoire

To a stirred solution of 1-(2-pyrimidinyl)-4-piperazinyl propanol 3 g. (0.013 mol) in 50 mol. of dimethylformamide was added 3.3 g. (0.013 mol) of diphenylmethylbromide and 2.9 g. (0.034 mol) of sodium bicarbonate. The reaction mixture was refluxed overnight, dimethylformamide was evaporated under reduced pressure, and the residue was extracted with methylene chloride (400 ml.). The methylene chloride extracts were collected, washed with water and evaporated, and the remaining residue was purified by HPLC to give 1.3 g. (26% yield) of the title compound. The free base which was converted to the (1:1) fumarate salt; m.p 166°-168° C.

Source

DOI: 10.6084/m9.figshare.5104873.v1Brevet: US04766215uspto-grants-1988_08