Reaktion #353909

Reaktionsgleichung

4-(piperazin-1-yl)anisole

4-chloropyridine hydrochloride

ammonia

→

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

Ausbeute 31.0%

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated at 160°-170° C. (bath temperature) for 7 minutes
2. 2
   SonstigeThe solid obtained
3. 3
   Temperaturon cooling
4. 4
   ExtraktionThe solid precipitate was extracted into ethyl acetate
5. 5
   Extraktionthe organic extract
6. 6
   Waschenwashed with water
7. 7
   Filtrationfiltered through phase
8. 8
   Sonstigeseparating paper (Whatman 1PS)
9. 9
   Sonstigeevaporated
10. 10
    SonstigeThe residue was recrystallised from ethanol

Vorschrift

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) δ 8.3(2H,d); 6.86(4H,m); 6.71(2H,d); 3.78(3H,s); 3.46(4H,m); 3.2(4H,m).

Quelle