反应详情

To a solution 3-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]propanol (1.81 g, 6.5 mmol) triethylamine (0.9 g, 9.0 mmol) in DCM (45 ml) was added decanoyl chloride (1.5 g, 7.8 mmol) dropwise at room temperature. The mixture was stirred for 20 minutes, then concentrated down to a crude solid. The solid was extracted into EtOAc (20 ml), and the insoluble salts were filtered. The EtOAc was removed. The crude oil was purified by flash choursomatography (Sorbsil C-30, 30 g; eluted with MeOH:DCM). The oil thus obtained (2.54 g, 90%) was converted to a fumarate salt with fumaric acid (670 mg) in ethanol. The crystals collected weighed 1.61 g, m.p.=100°-102° C.

1. concentrationconcentrated down to a crude solid
2. extractionThe solid was extracted into EtOAc (20 ml)
3. filtrationthe insoluble salts were filtered
4. customThe EtOAc was removed
5. customThe crude oil was purified by flash choursomatography (Sorbsil C-30, 30 g; eluted with MeOH:DCM)
6. customThe oil thus obtained (2.54 g, 90%)
7. customThe crystals collected