反应详情

温度

0 °C

2-Bromo-N-(2-tert-butyl-5-nitro-phenyl)-acetamide (Step B, 80 g, 253 mmol) and K2CO3 (70 g, 506 mmol) were combined in a 3 L 3-neck round bottom flask fitted with a mechanical stirrer, N2(g) inlet, and pressure equalizing addition funnel. THF (1.75 L) was added and the mixture cooled to 0° C. under N2(g). N,N-Dimethylamine (400 mL of a 2 M solution in THF, 800 mmol) was added to the mixture through the pressure equalizing addition funnel over 30 min. The mixture was gradually warmed to RT with stirring overnight. The reaction was quenched by filtering under vacuum and concentrating the filtrate under reduced pressure. The recovered material was eluted through a 36×7 cm column of silica gel with 50% EtOAc:Hexanes giving a brown solid.

1. customfitted with a mechanical stirrer, N2(g) inlet
2. additionaddition funnel
3. additionaddition funnel over 30 min
4. temperatureThe mixture was gradually warmed to RT
5. customThe reaction was quenched
6. filtrationby filtering under vacuum
7. concentrationconcentrating the filtrate under reduced pressure
8. washThe recovered material was eluted through a 36×7 cm column of silica gel with 50% EtOAc