Reaktion #2337

Reaktionsgleichung

product

4-[4-[4-(4-pyridyl)piperazin-1-yl]phenoxy]butyric acid

methanol

pyridine hydrochloride

→

title compound

Ausbeute 81.3%

4-[4-[4-(4-pyridyl)piperazin-1-yl]phenoxy]butyric acid, hydrochloride salt

Ausbeute 81.3%

Lösungsmittel

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturto reflux
3. 3
   TemperaturHeating
4. 4
   SonstigeThe reaction mixture was evaporated until a slight turbidity
5. 5
   SonstigeOn further cooling, a precipitate formed which
6. 6
   Sonstigewas collected
7. 7
   Waschenwashed with ethyl acetate
8. 8
   Sonstigedried

Vorschrift

A mixture of the product from Example 26 (1.5 g) and methanol (80 ml) was heated to reflux with stirring, and solid pyridine hydrochloride (0.5 g) was added. Heating was stopped and ethyl acetate (10 ml) was added. The reaction mixture was evaporated until a slight turbidity was observed. On further cooling, a precipitate formed which was collected, washed with ethyl acetate and dried to give the title compound (1.33 g) as a beige solid: m.p.>240° C. (dec); NMR (d6 -DMSO) δ 1.90 (2H, m), 2.36 (2H, t), 3.17 (4H, m), 3.83 (4H, m), 3.91 (2H, t), 6.89 (4H, q), 7.26 (2H, d), 8.25 (2H, d), 12.1 (1H, br), 13.75 (1H, br); m/Z 342 (M+H)+ ; calculated for C19H23N3O3. 1.0 HCl: C, 60.4%; H, 6.4%; N, 11.1%; found: C, 60.0%; H, 6.4%, N, 10.8%.

Quelle