反应详情

1-Cyclobutyl-4-(4-piperidinylmethyl)piperidine (may be prepared as described in Description 6) (0.50 g), 1,1-dimethylethyl 5-bromo-2-pyridinecarboxylate (may be prepared as described in Description 12) (0.66 g), BINAP (0.15 g) and Cs2CO3 (1.6 g) were added to toluene (20 ml) under argon and the reaction mixture degassed by sequential freezing in dry ice followed by warming to room temp under vacuum (3×). After stirring for 5 min Pd(OAc)2 (0.05 g) was added and the reaction mixture heated at 80° C. for 20 h. The reaction mixture was filtered and evaporated, after which chromatography (silica gel, eluting with methanol/dichloromethane, 0-20%) afforded the title compound (E3) as a solid (0.23 g). MS electrospray (+ion) 414 (MH+)

1. customthe reaction mixture degassed by sequential freezing in dry ice
2. additionwas added
3. temperaturethe reaction mixture heated at 80° C. for 20 h
4. filtrationThe reaction mixture was filtered
5. customevaporated
6. washafter which chromatography (silica gel, eluting with methanol/dichloromethane, 0-20%)