Реакция #63648

ord-aa5a0f291e6b415aaae345a373a5758e

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ТемператураThe reaction mixture was refluxed overnight
  2. 2
    Другоеdimethylformamide was evaporated under vacuum
  3. 3
    Экстракцияthe residue was extracted with methylene chloride (3×400 ml.)
  4. 4
    ДругоеThe methylene chloride extracts were collected
  5. 5
    Промывкаwashed with water
  6. 6
    Сушкаdried (anhydrous Na2SO4)
  7. 7
    ДругоеEvaporation of the methylene chloride

Методика

To a stirred solution of 1-(6-chloro-2-pyrazinyl)-4-piperazinyl propanol 3 g. (0.013 mol) in 50 ml. of dimethylformamide was added 3.3 g. (0.017 mol) of bis(4-fluorophenyl)methylbromide and 2.6 g. (0.034 mol) of sodium bicarbonate. The reaction mixture was refluxed overnight, dimethylformamide was evaporated under vacuum and the residue was extracted with methylene chloride (3×400 ml.). The methylene chloride extracts were collected, washed with water and dried (anhydrous Na2SO4). Evaporation of the methylene chloride afforded the title compound as a brown oil. HPLC purification afforded 2 g. (37% yield) of the pure product. It was converted to the (1:1) fumarate salt and recovered as the hemihydrate; m.p. 165°-167° C.

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US04766215uspto-grants-1988_08