反应详情

A 2 L, 3 necked round bottomed flask equipped with a mechanical stirrer, thermocouple and ice-bath was charged with concentrated H2SO4(aq) (635 mL) and concentrated HNO3(aq) (62 mL). The flask and its contents were cooled to 0° C. (4-Bromo-phenyl)-(3-nitro-phenyl)-methanone (127 g, 0.42 mol) was added over a period of 1 h and the temperature was kept under 10° C. Thirty minutes later, the reaction was complete by thin layer chromatographic analysis (Hexanes/EtOAc 6:4). The reaction was poured into ice-H2O (2 L). The solids were filtered, washed with H2O (4 L), saturated NaHCO3(aq) (1 L) and an additional portion of H2O (1 L). The product was dried at 45° C., for 48 h yielding (4-Bromo-3-nitro-phenyl)-(3-nitro-phenyl)-methanone in 95% (138.4 g, 0.39 mol).

1. customA 2 L, 3 necked round bottomed flask equipped with a mechanical stirrer
2. additionwas added over a period of 1 h
3. customwas kept under 10° C
4. customThirty minutes
5. filtrationThe solids were filtered
6. washwashed with H2O (4 L), saturated NaHCO3(aq) (1 L)
7. customThe product was dried at 45° C., for 48 h