反应 #2303

反应方程式

4-(piperazin-1-yl)anisole

4-chloropyridine hydrochloride

ammonia

→

4-[4-(4-pyridyl)-piperazin-1-yl]anisole

收率 31.0%

溶剂

water

反应条件

后处理

1. 1
   温度heated at 160°-170° C. (bath temperature) for 7 minutes
2. 2
   其他The solid obtained
3. 3
   温度on cooling
4. 4
   萃取The solid precipitate was extracted into ethyl acetate
5. 5
   萃取the organic extract
6. 6
   洗涤washed with water
7. 7
   过滤filtered through phase
8. 8
   其他separating paper (Whatman 1PS)
9. 9
   其他evaporated
10. 10
    其他The residue was recrystallised from ethanol

实验过程

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).

来源