反应详情

温度

120 °C

In a 350 mL pressure flask, 2-fluoro-5-nitroaniline (10 g, 0.064 mol), methylamine as a 2M solution in THF (65 mL, 0.13 mol) and potassium carbonate (18 g, 0.13 mol) in 1-Methyl-2-pyrrolidinone (80 mL) were combined. The flask was sealed and heated to 120 degrees C. overnight. The reaction was monitored by TLC. When reaction was judged to be complete based upon consumption of 2-fluoro-5-nitroaniline, it was cooled to room temperature and poured into 2-3 times the total reaction volume of water. When a precipitate was formed, it was filtered and dried. The product was carried on without purification. 1H NMR (300 MHz, d6DMSO) δ 7.54 (dd, J=8.79, 2.64 Hz, 1H), 7.39 (d, J≦2.64 Hz, 1H), 6.41 (d, J=8.79 Hz, 1H), 6.11 (d, J=4.39 Hz, 1H), 5.07 (s, 2H), 2.83 (d, 1H), 4.83 Hz, 3H).

1. customThe flask was sealed
2. customovernight
3. customWhen reaction
4. customto be complete based upon consumption of 2-fluoro-5-nitroaniline, it
5. temperaturewas cooled to room temperature
6. additionpoured into 2-3 times the total reaction volume of water
7. customWhen a precipitate was formed
8. filtrationit was filtered
9. customdried
10. customThe product was carried on without purification