반응 #2337

반응 방정식

product

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

methanol

pyridine hydrochloride

→

title compound

수율 81.3%

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

수율 81.3%

용매

ethyl acetate

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도to reflux
3. 3
   온도Heating
4. 4
   기타The reaction mixture was evaporated until a slight turbidity
5. 5
   기타On further cooling, a precipitate formed which
6. 6
   기타was collected
7. 7
   세척washed with ethyl acetate
8. 8
   기타dried

실험 절차

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%.

출처