反応 #2303

反応方程式

4-(piperazin-1-yl)anisole

4-chloropyridine hydrochloride

ammonia

→

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

収率 31.0%

溶媒

water

反応条件

後処理

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

実験手順

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).

出典