Potassium Carbonate → HCID 21960114, compound

Participants

Reaction Steps

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.

Provenance & Evidence