反应详情

A mixture of 6-fluoro-3-(4-piperidinyl)-1,2-benzisoxazole (3.75 g, 17 mmol), K2CO3 (3 g, 21.7 mmol), bromoethyl methyl ether (2.84 g, 20.4 mmol) in acetonitrile (150 ml) was heated at reflux for 3.5 hours. The reaction was cooled. The inorganics were filtered and rinsed with DCM. The organic solution was concentrated down to an oil (7 g). Purification on a flash chromatography column (SiO2, 45 g; eluted with methanol/DCM) gave a light yellow oil as product (4 g, 87%). This oil was dissolved into ethanol and treated with a solution of fumaric acid (1.67 g) in ethanol (20 ml). White crystals (5.15 g) were collected, m.p.=157°-158° C.

1. temperaturewas heated
2. temperatureat reflux for 3.5 hours
3. temperatureThe reaction was cooled
4. filtrationThe inorganics were filtered
5. washrinsed with DCM
6. concentrationThe organic solution was concentrated down to an oil (7 g)
7. customPurification
8. washon a flash chromatography column (SiO2, 45 g; eluted with methanol/DCM)
9. customgave a light yellow oil as product (4 g, 87%)
10. customWhite crystals (5.15 g) were collected