反応 #83915

反応方程式

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

溶媒

acetonitrile

DCM

反応条件

後処理

1. 1
   温度was heated
2. 2
   温度at reflux for 24 hours
3. 3
   ろ過filtered
4. 4
   濃縮The solvent was concentrated to an oil (~7.1 g)
5. 5
   その他Purification
6. 6
   洗浄on a silica gel column (55 g, SiO2, eluted with MeOH:DCM)
7. 7
   その他yielded a solid product
8. 8
   その他Recrystallization from hot ethanol
9. 9
   その他yielded 2.1 g (48%), m.p.=131°-132° C.

実験手順

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.

出典