反应 #83965

反应方程式

3-(4-piperidinyl)-6-fluorobenzisoxazole

K2CO3

3-(2-chloroethyl)-2-methyl-3H-4-quinazolinone

→

3-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-2-methyl-3H-quinazolin-4-one

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度at reflux for 16 hours
3. 3
   过滤The solids were filtered
4. 4
   其他the solvent was evaporated
5. 5
   其他The residue was purified over a flash chromatography column (SiO2, 75 gm, eluted with dichloromethane and MeOH in dichloromethane)
6. 6
   其他The pure product thus obtained
7. 7
   其他Recrystallization from ethanol yielded white crystals, 3.94 gm (53%), m.p. 164°-165° C

实验过程

A stirred mixture of 3-(4-piperidinyl)-6-fluorobenzisoxazole (4 g, 18.2 mmol), K2CO3 (3.76 g, 27.2 mmol) and 3-(2-chloroethyl)-2-methyl-3H-4-quinazolinone (6.0 g, 27 mmol) in acetonitrile (300 ml) was heated at reflux for 16 hours. The reaction was complete as judged by TLC. The solids were filtered and the solvent was evaporated. The residue was purified over a flash chromatography column (SiO2, 75 gm, eluted with dichloromethane and MeOH in dichloromethane). The pure product thus obtained weighed 6.5 gm. Recrystallization from ethanol yielded white crystals, 3.94 gm (53%), m.p. 164°-165° C. This material appeared pure by TLC over silica gel plates.

来源