반응 #83984

반응 방정식

4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine

K2CO3

2-toluenesulfonyl-2-phenyl-1,3-indandione

acetonitrile

→

2-[2-[4-(6-Fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethyl]-2-phenyl-1,3-indandione

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 3 hours
3. 3
   온도The mixture was cooled
4. 4
   여과the insolubles were filtered
5. 5
   기타The solvent was removed on a rotary evaporator
6. 6
   기타The residue was purified twice
7. 7
   세척a flash chromatography column (SiO2, 45 g and 40 g; eluted with DCM)
8. 8
   기타The product thus purified
9. 9
   기타was recrystallized from ethanol (30 ml) and isopropyl ether, yield: 2.8 g, m.p. 149°-150° C.

실험 절차

A mixture of 4-(6-fluoro-1,2-benzisoxazol-3-yl)piperidine (2.2 g, 10 mmol), K2CO3 (1.6 g, 11.6 mmol) and 2-toluenesulfonyl-2-phenyl-1,3-indandione (4.2 g, 10 mmol) in acetonitrile (50 ml) was heated at reflux for 3 hours. The mixture was cooled and the insolubles were filtered. The solvent was removed on a rotary evaporator. The residue was purified twice using a flash chromatography column (SiO2, 45 g and 40 g; eluted with DCM). The product thus purified was recrystallized from ethanol (30 ml) and isopropyl ether, yield: 2.8 g, m.p. 149°-150° C.

출처