反应详情

To a mixture of 4-[4-(6-fluoro-1,2-benzisoxazol-3yl)-1-piperidinyl]-2-methyl-2-butanol (4.68 g, 15.3 mmol) and triethylamine (2.23 g, 22.3 mmol) in chloroform (20 ml) was added decanoyl chloride (3.5 g, 18.4 mmol, 1.2 eq) dropwise at 0° C. The reaction was stirred at ambient temperature for 4 hours. The solvent was removed. The residue was purified by flash chromatography over a silica gel column (SiO2, 65 g, eluted with DCM, 1 l, 1% CH3OH in DCM, 1 l). The product thus purified weighed 5.7 g (80%) as an oil. This oily product was converted to the fumarate salt in ethanol with fumaric acid (1.51 g, 1.0 eq) to yield 3.34 g, m.p.=133°-134° C.

1. customThe solvent was removed
2. customThe residue was purified by flash chromatography over a silica gel column (SiO2, 65 g, eluted with DCM, 1 l, 1% CH3OH in DCM, 1 l)
3. customThe product thus purified
4. customto yield 3.34 g, m.p.=133°-134° C.