反应详情

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (2.2 g, 10 mmol), K2CO3 (3 g), 1-[4-(3-bromopropoxy)-3-methoxyphenyl]pentanone (3.7 g, 11.3 acetonitrile (140 ml) was heated at reflux for 4 hours. At the end of the reaction, the mixture was cooled and filtered. The filtrate was concentrated to an oil. Purification was performed by flash chromatography over a silica gel column (SiO2, 55 g; eluted with 1% methanol in dichloromethane, 600 mi; 3% methanol: 97% dichloromethane, 400 ml). The fractions containing pure product were pooled and concentrated to a solid (4.3 g, 91%). Recrystallization from ethanol (10 ml) gave a powdery solid of 1-[4-[3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propoxy]-3-methoxyphenyl]pentanone (3.22 g), m.p.=79°-80° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. customAt the end of the reaction
4. temperaturethe mixture was cooled
5. filtrationfiltered
6. concentrationThe filtrate was concentrated to an oil
7. customPurification
8. washwas performed by flash chromatography over a silica gel column (SiO2, 55 g; eluted with 1% methanol in dichloromethane, 600 mi; 3% methanol: 97% dichloromethane, 400 ml)
9. additionThe fractions containing pure product
10. concentrationconcentrated to a solid (4.3 g, 91%)
11. customRecrystallization from ethanol (10 ml)