反应详情

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.0 g, 13.6 mmol), K2CO3 (3.5 g, 25 mmol), 2-bromoethyl acetate (4 g, 26.5 mmol) in acetonitrile (50 ml) was heated at reflux for 4 hours. After cooling to room temperature, the inorganic salts were filtered and washed with DCM (dichloromethane 50 ml). The organic solvent was removed on a rotary evaporator to give an oil. The oily product was purified on a flash chromatography column (60 g of SiO2 ; eluted with MeOH 2%-4% in DCM). The pure product thus obtained weighed 4.43 g. This oil was dissolved in ethanol and treated with a solution of fumaric acid (1.2 g) in ethanol. The salt crystallized out at room temperature to yield 3.44 g (57%), m.p.=154°-155° C.

1. temperaturewas heated
2. temperatureat reflux for 4 hours
3. filtrationthe inorganic salts were filtered
4. washwashed with DCM (dichloromethane 50 ml)
5. customThe organic solvent was removed on a rotary evaporator
6. customto give an oil
7. customThe oily product was purified on a flash chromatography column (60 g of SiO2 ; eluted with MeOH 2%-4% in DCM)
8. customThe pure product thus obtained
9. customThe salt crystallized out at room temperature
10. customto yield 3.44 g (57%), m.p.=154°-155° C.