反应详情

温度

100 °C

To a mixture of 5-bromo-2-nitropyridine (406 mg, 2 mmol) and 1-acetylpiperazine (256 mg, 2 mmol) in toluene (5 mL) is added Cs2CO3, then Pd2(dba)3 (74 mg, 0.08 mmol) and BINAP (100 mg, 0.16 mmol) are added. The mixture is degassed, and heated at 100° C. for 16 hours. Then the mixture is cooled down to room temperature, diluted with EtOAc, and filtered through celite. The filtrate is concentrated under reduced pressure. The crude product is purified by column chromatography (SiO2, MeOH:CH2Cl2=0.7:99.3 to 6:93) to give 270 mg of the title compound as yellow solid.

1. customThe mixture is degassed
2. temperatureThen the mixture is cooled down to room temperature
3. additiondiluted with EtOAc
4. filtrationfiltered through celite
5. concentrationThe filtrate is concentrated under reduced pressure
6. customThe crude product is purified by column chromatography (SiO2, MeOH:CH2Cl2=0.7:99.3 to 6:93)