反应详情

温度

70 °C

A solution of 1,2,3-trifluoro-4-nitrobenzene (1) (1.00 g, 5.64 mmol, 1.00 equiv) in methanolic ammonia (1.5 mL) was taken in microwave vial and heated to 70° C. for 90 min in the microwave. The solvent was evaporated under vacuum to give crude; which was purified by silica gel column chromatography (EtOAc/Hexane 1:49) to furnish compound 2 (0.350 g, 35.6%) as yellow solid. TLC: 10% EtOAc/Hexane (Rf: 0.10); 1H NMR (500 MHz, DMSO-d6): δ 7.94-7.91 (m, 1H), 7.51 (s, 2H), 6.75-6.70 (m, 1H); LC-MS: m/z=173 (M+-1) at RT 3.15 (99.8% purity)

1. customThe solvent was evaporated under vacuum
2. customto give crude
3. customwhich was purified by silica gel column chromatography (EtOAc/Hexane 1:49)