반응 #2303
ord-61aad68a3b1947e1aaa4cb73733b890c
반응 방정식
4-(piperazin-1-yl)anisole
4-chloropyridine hydrochloride
ammonia
→
4-[4-(4-pyridyl)-piperazin-1-yl]anisole
수율 31.0%
용매
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도heated at 160°-170° C. (bath temperature) for 7 minutes
- 2기타The solid obtained
- 3온도on cooling
- 4추출The solid precipitate was extracted into ethyl acetate
- 5추출the organic extract
- 6세척washed with water
- 7여과filtered through phase
- 8기타separating paper (Whatman 1PS)
- 9기타evaporated
- 10기타The 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).