反应 #83893

反应方程式

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

K2CO3

2-methanesulfonyloxymethyl-1,4-benzodioxan

→

2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]methyl-1,4-benzodioxan

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 12 hours
3. 3
   其他At the end of the reaction
4. 4
   过滤the insolubles were filtered
5. 5
   洗涤rinsed with dichloromethane
6. 6
   浓缩The organic solution was concentrated
7. 7
   其他The crude oil was purified by flash chromatography on a silica gel column
8. 8
   workup.ADDITIONThe fractions containing the pure product
9. 9
   浓缩concentrated to a light yellow oil (3.94 g, 74%)
10. 10
    其他Crystallization from ethanol and petroleum ether

实验过程

A stirred mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), K2CO3 (2.45 g, 17.7 mmol), 2-methanesulfonyloxymethyl-1,4-benzodioxan (3.35 g, 13.7 mmole) in acetonitrile (100 ml) was heated at reflux for 12 hours. At the end of the reaction, the insolubles were filtered and rinsed with dichloromethane. The organic solution was concentrated. The crude oil was purified by flash chromatography on a silica gel column. The fractions containing the pure product were pooled and concentrated to a light yellow oil (3.94 g, 74%). Crystallization from ethanol and petroleum ether gave 2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]methyl-1,4-benzodioxan as off-white crystals, 2.22 g, m.p.=86°-87° C.

来源