反应详情

A mixture of tert-butyl 2,8-diazaspiro[4.5]decane-2-carboxylate (2.5 mmol, 1.0 eq.) and 4-bromo-8-(trifluoromethyl)quinoline (2.5 mmol, 1.0 eq.) and tBuONa (7.5 mmol, 3.0 eq.) in toluene (12 ml) was degassed with argon for 10 min. BINAP (0.15 mmol, 0.06 eq.) and Pd(OAc)2 (0.05 mmol, 0.02 eq.) were added and the reaction mixture obtained was heated under reflux for 14 h. The reaction mixture was filtered over Celite and the filtrate was concentrated in vacuo in order to obtain the crude product, which was purified by column chromatography (silica gel, 22-25% ethyl acetate in hexane), in order to obtain the desired product. Yield: 40%

1. customwas degassed with argon for 10 min
2. customthe reaction mixture obtained
3. temperaturewas heated
4. temperatureunder reflux for 14 h
5. filtrationThe reaction mixture was filtered over Celite
6. concentrationthe filtrate was concentrated in vacuo in order
7. customto obtain the crude product, which
8. customwas purified by column chromatography (silica gel, 22-25% ethyl acetate in hexane), in order