Reacción #83915

Ecuación de reacción

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

Disolventes

acetonitrile

DCM

Condiciones de reacción

Tratamiento posterior

1. 1
   Temperaturawas heated
2. 2
   Temperaturaat reflux for 24 hours
3. 3
   Filtraciónfiltered
4. 4
   ConcentraciónThe solvent was concentrated to an oil (~7.1 g)
5. 5
   OtroPurification
6. 6
   Lavadoon a silica gel column (55 g, SiO2, eluted with MeOH:DCM)
7. 7
   Otroyielded a solid product
8. 8
   OtroRecrystallization from hot ethanol
9. 9
   Otroyielded 2.1 g (48%), m.p.=131°-132° C.

Procedimiento

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.

Fuente