反应详情

温度

5 °C

To a solution of 2,4-difluoroaniline (0.394 mL, 3.87 mmol) in concentrated sulfuric acid (5 mL, 94 mmol) at 0° C. was added drop wise nitric acid (0.272 mL, 375 mg, 3.87 mmol) in 20 min. The reaction was stirred under 5° C. for 30 min. The reaction mixture was poured in ice cold water and extracted with ether. Organic layer was washed with saturated NaHCO3 solution, dried and evaporated to give 2,4-difluoro-5-nitroaniline 71 (467 mg, 69.3%). NMR (400 MHz, CDCl3) 3.91 (br s, 2H), 6.98 (t, J=10.2 Hz, 1H), 7.51 (dd, J=8.6 Hz and 7.0 Hz, 1H).

1. additionThe reaction mixture was poured in ice cold water
2. extractionextracted with ether
3. washOrganic layer was washed with saturated NaHCO3 solution
4. customdried
5. customevaporated