反应详情

4-(Benzofurazan-5-carbonyl)piperidine hydrochloride (80 mg, 0.3 mmol), 5-(2-bromoethyl)benzofurazan (170 mg, 0.75 mmol), sodium bicarbonate (101 mg, 1.2 mmol) and lithium iodide (1 mg) in ethanol were heated under reflux for 19 hours, cooled and the solvent was evaporated under reduced pressure. The residue was purified by flash column chromatography on silica gel, eluting with CH2Cl2 /CH3OH/NH3 (Aq.); 98:2:0.2 to give a yellow solid. This was dissolved in ethyl acetate (2 ml), and ethanolic HCl (Ca. 1M, 1 ml) was added. The resulting solid was collected and dried in vacuo to give the hydrochloride as a white solid (50 mg, 40%), mp 226°-228° C.

1. temperatureunder reflux for 19 hours
2. temperaturecooled
3. customthe solvent was evaporated under reduced pressure
4. customThe residue was purified by flash column chromatography on silica gel
5. washeluting with CH2Cl2 /CH3OH/NH3 (Aq.)
6. custom98:2:0.2 to give a yellow solid
7. customThe resulting solid was collected
8. customdried in vacuo