反应 #83888

反应方程式

6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole

N,N-dimethyl-4-bromopropoxy-3-methoxybenzamide

K2CO3

→

N,N-dimethyl-4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3methoxybenzamide

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for one hour
3. 3
   其他At the end of the reaction
4. 4
   过滤the insolubles were filtered
5. 5
   洗涤washed with dichloromethane
6. 6
   其他The solvent was removed on a rotary evaporator
7. 7
   其他The residue was purified by flash chromatography over a silica gel column
8. 8
   其他The product thus obtained as an oil
9. 9
   其他Crystallization from hot ethanol (45 ml)

实验过程

A stirred mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.9 g, 17.7 mmol), N,N-dimethyl-4-bromopropoxy-3-methoxybenzamide (5.54 g, 17.5 mmol) and K2CO3 (3 g) in acetonitrile (250 ml) was heated at reflux for one hour. At the end of the reaction, the insolubles were filtered and washed with dichloromethane. The solvent was removed on a rotary evaporator. The residue was purified by flash chromatography over a silica gel column. The product thus obtained as an oil weighed 7 g. Crystallization from hot ethanol (45 ml) afforded analytically pure N,N-dimethyl-4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3methoxybenzamide, 3.95 g, 50%, as light yellow crystals, m.p.=126°-127° C.

来源