反应详情

温度

90 °C

In a oven-dried flask and under a nitrogen atmosphere, were placed 3,5-dibromonitrobenzene (500 mg, 1.78 mmol), (+/−) BINAP (110 mg, 0.1 eq), Cs2CO3 (1.62 g, 3 eq), Pd2dba3 (81 mg, 0.11 eq) and 10 mL of dry 1,4-dioxane. N-Methylpiperazine (0.47 mL, 2.4 eq) was added and the mixture was stirred at 90° C. for 48 h. The solution was filtered through a celite pad and evaporated. The residue was purified by flash chromatography on silica gel (DCM/MeOH/NH4OH//95/5/1) to yield expected compound as an orange solid (258 mg, 45% yield). m/z (MALDI-TOF) 320.2 [M+H]+;

1. customIn a oven-dried flask and under a nitrogen atmosphere, were placed
2. filtrationThe solution was filtered through a celite pad
3. customevaporated
4. customThe residue was purified by flash chromatography on silica gel (DCM/MeOH/NH4OH//95/5/1)