反应详情

A mixture of 2-[4-(6-fluoro-1,2-benzisoxazol-3-yl)-1-piperidinyl]ethylamine (1.52 g, 5.73 mmol), 1,2-dibromo-4-(triisopropylsilyl)oxy-xylene (2.4 g,(1.8 g, 13 mmol) K2CO3 (1.8 g, 13 mmol) in acetonitrile (300 ml) was stirred overnight (18 hours) at room temperature. The mixture was filtered and the solvent was stripped. The residue was purified by flash chromatography over a silica gel column (7 gm of SiO2 ; eluted with 1-3% CH3OH in dichloromethane. The product thus purified (weight: 900 mg) was converted to the fumarate salt by treatment with fumaric acid (194 mg) in hot ethanol. The crystals were collected and weighed 590 mg, m.p. 208°-210° C.

1. filtrationThe mixture was filtered
2. customThe residue was purified by flash chromatography over a silica gel column (7 gm of SiO2
3. washeluted with 1-3% CH3OH in dichloromethane
4. customThe product thus purified (weight: 900 mg)
5. customThe crystals were collected