反应详情

温度

100 °C

1-isopropylpiperazine (1.29 g, 5.66 mmol) and tert-butyl (4-bromo-2-nitrophenyl)carbamate (1.5 g, 4.71 mmol) were taken in a mixture of dry toluene (15 mL) and dioxane (2 mL) in a seal tube under argon atmosphere at room temperature. The Argon gas was purged for 5-10 min. Then Cs2CO3 (3.06 g, 9.43 mmol) and Xantphos (0.54 g, 0.94 mmol) were added and the resulting reaction mixture was purged with argon gas for 5 min., followed by Pd2(dba)3 (0.43 g, 0.47 mmol). The argon gas purging was continued for additional 5 min. before sealing the reaction vial. Then the reaction mixture was heated at 100° C. for 12 hr. After completion of the reaction by TLC, the reaction mixture was cooled to room temperature, filtered through celite bed and concentrated. The residue was purified by silica gel column chromatography (DCM:MeOH/97:3) to afford the title compound (1.2 g, yield: 70.5%). MS (ESI): 365.5 [M+H]+.

1. customThe Argon gas was purged for 5-10 min
2. customthe resulting reaction mixture
3. customwas purged with argon gas for 5 min.
4. customThe argon gas purging
5. customAfter completion of the reaction by TLC
6. temperaturethe reaction mixture was cooled to room temperature
7. filtrationfiltered through celite bed
8. concentrationconcentrated
9. customThe residue was purified by silica gel column chromatography (DCM:MeOH/97:3)