Реакция #2303

ord-61aad68a3b1947e1aaa4cb73733b890c

Растворители

Условия реакции

Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    Температураheated at 160°-170° C. (bath temperature) for 7 minutes
  2. 2
    ДругоеThe solid obtained
  3. 3
    Температураon cooling
  4. 4
    ЭкстракцияThe solid precipitate was extracted into ethyl acetate
  5. 5
    Экстракцияthe organic extract
  6. 6
    Промывкаwashed with water
  7. 7
    Фильтрацияfiltered through phase
  8. 8
    Другоеseparating paper (Whatman 1PS)
  9. 9
    Другоеevaporated
  10. 10
    ДругоеThe residue was recrystallised from ethanol

Методика

4-(piperazin-1-yl)anisole (4.24 g) and 4-chloropyridine hydrochloride (3.35 g) were intimately mixed and heated at 160°-170° C. (bath temperature) for 7 minutes. The solid obtained on cooling was dissolved in water (75 ml) and the solution basified with aqueous ammonia. The solid precipitate was extracted into ethyl acetate and the organic extract washed with water, filtered through phase separating paper (Whatman 1PS) and evaporated. The residue was recrystallised from ethanol to give 4-[4-(4-pyridyl)-piperazin-1-yl]anisole (1.84 g) as a solid: m.p. 165°-167° C.; NMR (CDCl3) δ8.3(2H,d); 6.86(4H,m); 6.71(2H,d); 3.78(3H,s); 3.46(4H,m); 3.2(4H,m).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US05728701uspto-grants-1998_03