반응 #83915

반응 방정식

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

2-chloroethyl morpholine hydrochloride

K2CO3

→

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

용매

acetonitrile

DCM

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도at reflux for 24 hours
3. 3
   여과filtered
4. 4
   농축The solvent was concentrated to an oil (~7.1 g)
5. 5
   기타Purification
6. 6
   세척on a silica gel column (55 g, SiO2, eluted with MeOH:DCM)
7. 7
   기타yielded a solid product
8. 8
   기타Recrystallization from hot ethanol
9. 9
   기타yielded 2.1 g (48%), m.p.=131°-132° C.

실험 절차

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), 2-chloroethyl morpholine hydrochloride (4.46 g, 29.7 mmol) and K2CO3 (7.3 g, 2.2 eq) in acetonitrile (60 ml) was heated at reflux for 24 hours. The crude mixture was diluted with DCM and filtered. The solvent was concentrated to an oil (~7.1 g). Purification on a silica gel column (55 g, SiO2, eluted with MeOH:DCM) yielded a solid product weighing 4 g. Recrystallization from hot ethanol yielded 2.1 g (48%), m.p.=131°-132° C.

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