반응 #83965

반응 방정식

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

용매

acetonitrile

반응 조건

후처리

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

실험 절차

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.

출처