反应详情

温度

20 °C

Conc. nitric acid (15.8 mL, 376.9 mmol) was added to a solution of 4-bromoaniline (40 g, 232.5 mmol) in H2SO4/CH2Cl2 (400 mL, 1:1, v/v) dropwise at 0° C. under an atmosphere of N2. The cooling bath was removed and the mixture was stirred at 20° C. until the starting material was consumed (about 1 h). The reaction mixture was poured onto water and neutralized with NaOH solution to pH=9 and extracted with DCM. The organic layer was dried, filtered and evaporated in vacuo to afford the crude product 4-bromo-3-nitro-aniline, which was used directly in the next step.

1. customdropwise at 0° C.
2. customThe cooling bath was removed
3. customwas consumed (about 1 h)
4. additionThe reaction mixture was poured onto water and neutralized with NaOH solution to pH=9
5. extractionextracted with DCM
6. customThe organic layer was dried
7. filtrationfiltered
8. customevaporated in vacuo