反应详情

温度

-7.5 °C

2-Bromo-4-tert-butyl-phenylamine (162 g, 0.71 mol) was added dropwise to H2SO4 (410 mL) at room temperature to yield a clear solution. This clear solution was then cooled down to −5 to −10° C. A solution of KNO3 (82.5 g, 0.82 mol) in H2SO4 (410 mL) was added dropwise while the temperature was maintained between −5 to −10° C. Upon completion, the reaction mixture was poured into ice/water and extracted with EtOAc. The combined organic layers were washed with 5% Na2CO3 and brine, dried over Na2SO4 and concentrated. The residue was purified by a column chromatography (EtOAc/petroleum ether 1/10) to give 2-bromo-4-tert-butyl-5-nitro-phenylamine as a yellow solid (152 g).

1. customto yield a clear solution
2. temperaturewas maintained between −5 to −10° C
3. extractionextracted with EtOAc
4. washThe combined organic layers were washed with 5% Na2CO3 and brine
5. dry with materialdried over Na2SO4
6. concentrationconcentrated
7. customThe residue was purified by a column chromatography (EtOAc/petroleum ether 1/10)