Reaktion #668725

Reaktionsgleichung

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

K2CO3

bromoethyl-1,3-dioxane

→

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

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturwas heated
2. 2
   Temperaturat reflux for 3 hours
3. 3
   FiltrationAt the end, the insolubles were filtered
4. 4
   Waschenrinsed with DCM
5. 5
   Sonstigethe filtrate was evaporated down
6. 6
   SonstigeThe crude mixture was purified by flash chromatography over a silica gel column (Sorbsil C-30, 25 g; eluted with DCM and MEOH (1-3%) in DCM)
7. 7
   workup.ADDITIONThe fractions containing the pure product with DCM and MEOH (1-3%) in DCM)
8. 8
   workup.ADDITIONThe fractions containing the pure product fumaric acid (1.0 g) ethanol solution
9. 9
   SonstigeThe crystals were collected

Vorschrift

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (2.0 g, 9.1 mmol), K2CO3 (1.5 g, 10.9 mmol) and bromoethyl-1,3-dioxane (2.1 g, 10.7 mmol) in acetonitrile (50 ml) was heated at reflux for 3 hours. At the end, the insolubles were filtered and rinsed with DCM and the filtrate was evaporated down. The crude mixture was purified by flash chromatography over a silica gel column (Sorbsil C-30, 25 g; eluted with DCM and MEOH (1-3%) in DCM). The fractions containing the pure product with DCM and MEOH (1-3%) in DCM). The fractions containing the pure product fumaric acid (1.0 g) ethanol solution. The crystals were collected: 3.98 g (77%), m.p.=161-162° C.

Quelle