反应详情

A mixture of 9-[5-ethoxy-(3-pyridyl)]-3-tert-butoxycarbonyl-3,9-diazabicyclo-[4.2.1]-nonane (0.23 g, 0.66 mmol), trifluoroacetic acid (0.75 g, 6.6 mmol) and dichloromethane (10 ml) was stirred for 3 days at room temperature. Sodium hydroxide (20 ml, 1M) was added and the phases were separated, followed by extraction with dichloromethane (20 ml). Chromatography on silica gel with dichloromethane, methanol and conc. ammonia (89:10:1) gave the title compound. The corresponding salt was obtained, by addition of a diethyl ether and methanol mixture (9:1) saturated with fumaric acid. Yield 0.39 g, 21%. Mp. 191-192° C.

1. customthe phases were separated
2. extractionfollowed by extraction with dichloromethane (20 ml)