反应详情

温度

5 °C

To a cold (0° C.) solution of 2-bromo-6-nitrotoluene (43.2 g, 0.2 mol) in con H2SO4 (600 mL) was added HNO3 (37 g, 0.24 mol) in small portions with efficient agitation while maintaining the temperature at 0-10° C. The reaction mixture was allowed to slowly warm to RT with stirring overnight then poured into crushed ice (1600 g). The solid was collected by filtration, thoroughly washed with water and dried in air. The crude material was recrystallised from EtOAc/hexanes to afford 40 g (77%) of 1-bromo-2-methyl-3,4-dinitrobenzene (154) as a pale white solid: MS (ESI) m/z=262 [M+1]+.

1. temperatureto slowly warm to RT
2. additionthen poured
3. filtrationThe solid was collected by filtration
4. washthoroughly washed with water
5. customdried in air
6. customThe crude material was recrystallised from EtOAc/hexanes