反应详情

tert-Butyl 3,8-diazabicyclo[3.2.1]octane-3-carboxylate hydrochloride (1.36 g, 5.5 mmol; see Preparation A) was dissolved in H2O/CHCl3/saturated K2CO3 solution (40:40:5) and the resulting mixture was shaken. The phases were separated, dried and evaporated giving 1.1 g (100%), of the free base. Acetonitrile (100 mL), 4-(2-bromoethoxy)benzonitrile (1.49 g, 6.6 mmol; from step (a) above) and K2CO3 (2.4 g, 17.5 mmol) were added. The mixture was stirred at 70° C. for 24 h, the solids were filtered off and the residue evaporated and purified by chromatography on silica, eluting with CHCl3:MeOH (95:5), to give 1.5 g (4.3 mmol) of the sub-title compound.

1. customPreparation A)
2. customThe phases were separated
3. customdried
4. customevaporated
5. customgiving 1.1 g (100%)
6. stirringThe mixture was stirred at 70° C. for 24 h
7. filtrationthe solids were filtered off
8. customthe residue evaporated
9. custompurified by chromatography on silica
10. washeluting with CHCl3:MeOH (95:5)