Реакция #83915

Уравнение реакции

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

Растворители

acetonitrile

DCM

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   Температураat reflux for 24 hours
3. 3
   Фильтрацияfiltered
4. 4
   КонцентрированиеThe solvent was concentrated to an oil (~7.1 g)
5. 5
   ДругоеPurification
6. 6
   Промывкаon a silica gel column (55 g, SiO2, eluted with MeOH:DCM)
7. 7
   Другоеyielded a solid product
8. 8
   ДругоеRecrystallization from hot ethanol
9. 9
   Другоеyielded 2.1 g (48%), m.p.=131°-132° C.

Методика

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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