反应 #2337

反应方程式

product

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

methanol

pyridine hydrochloride

→

title compound

收率 81.3%

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

收率 81.3%

溶剂

ethyl acetate

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度to reflux
3. 3
   温度Heating
4. 4
   其他The reaction mixture was evaporated until a slight turbidity
5. 5
   其他On further cooling, a precipitate formed which
6. 6
   其他was collected
7. 7
   洗涤washed with ethyl acetate
8. 8
   其他dried

实验过程

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%.

来源