تفاعل #83915

معادلة التفاعل

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

المذيبات

acetonitrile

DCM

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas heated
2. 2
   درجة الحرارةat reflux for 24 hours
3. 3
   ترشيحfiltered
4. 4
   تركيزThe solvent was concentrated to an oil (~7.1 g)
5. 5
   أخرىPurification
6. 6
   غسيلon a silica gel column (55 g, SiO2, eluted with MeOH:DCM)
7. 7
   أخرىyielded a solid product
8. 8
   أخرىRecrystallization from hot ethanol
9. 9
   أخرىyielded 2.1 g (48%), m.p.=131°-132° C.

الإجراء التجريبي

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.

المصدر