反応 #2337

反応方程式

product

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

methanol

pyridine hydrochloride

→

title compound

収率 81.3%

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

収率 81.3%

溶媒

ethyl acetate

反応条件

後処理

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

実験手順

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%.

出典