反应详情

To a solution of 4-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]butanol (2.0 g, 6.84 mmol), triethylamine (1,0 g, 10 mmol) in DCM (70 ml) decanoyl chloride (1.7 g, 8.9 mmol) was added dropwise at room temperature. The mixture was stirred for 1 hour., then was concentrated to a crude solid. The solid was extracted into ethyl acetate, and the insoluble salts were filtered. The solvents were removed. The crude product was purified by flash chromatography (Sorbsil C-30, 30 g, eluted with a mixture of MeOH in DCM). The oil thus obtained (2.5 g, 81%) was converted to a fumarate salt with fumaric acid (650 mg, 1.0 eq) in ethanol. Crystals were collected: 1.48 g, m.p.=109°-110° C.

1. concentration, then was concentrated to a crude solid
2. extractionThe solid was extracted into ethyl acetate
3. filtrationthe insoluble salts were filtered
4. customThe solvents were removed
5. customThe crude product was purified by flash chromatography (Sorbsil C-30, 30 g
6. washeluted with a mixture of MeOH in DCM)
7. customThe oil thus obtained (2.5 g, 81%)
8. customCrystals were collected