反应详情

温度

80 °C

A Pyrex tube was charged with sodium tert-butoxide (1.4 mmol), Pd2(dba)3 (0.00125 mmol), and BINAP (0.00375 mmol). The Pyrex tube was fitted with a septum and after the air atmosphere was replaced with argon, toluene (4 mL), 1-ethyl-6-iodo-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid ethyl ester (1.0 mmol), and benzophenone imine (1.2 mmol) were added by syringe. The reaction was sealed and heated to 80° C. with stirring until starting material was consumed as judged by GC analysis. The reaction mixture was cooled to room temperature, diluted with ether (40 mL), filtered, and concentrated. The crude reaction mixture was then recrystallized from MeOH to furnish the desired product in 90% yield.

1. customThe Pyrex tube was fitted with a septum
2. additionwere added by syringe
3. customThe reaction was sealed
4. customwas consumed
5. temperatureThe reaction mixture was cooled to room temperature
6. additiondiluted with ether (40 mL)
7. filtrationfiltered
8. concentrationconcentrated
9. customThe crude reaction mixture
10. customwas then recrystallized from MeOH