반응 #2303

ord-61aad68a3b1947e1aaa4cb73733b890c

반응 방정식

COc1ccc(N2CCNCC2)cc1
4-(piperazin-1-yl)anisole
Cl.Clc1ccncc1
4-chloropyridine hydrochloride
N
ammonia
COc1ccc(N2CCN(c3ccncc3)CC2)cc1
4-[4-(4-pyridyl)-piperazin-1-yl]anisole
수율 31.0%

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도heated at 160°-170° C. (bath temperature) for 7 minutes
  2. 2
    기타The solid obtained
  3. 3
    온도on cooling
  4. 4
    추출The solid precipitate was extracted into ethyl acetate
  5. 5
    추출the organic extract
  6. 6
    세척washed with water
  7. 7
    여과filtered through phase
  8. 8
    기타separating paper (Whatman 1PS)
  9. 9
    기타evaporated
  10. 10
    기타The residue was recrystallised from ethanol

실험 절차

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).

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US05728701uspto-grants-1998_03