反应详情

A solution of 1,2,3-trifluoro-4-nitrobenzene (5.0 g, 28.2 mmol) and ethanolamine (1.72 g, 28.2 mmol) in 100 ml of ethanol is stirred over night at room temperature then at 70° C. for 5 hours. The reaction is concentrated to dryness and purified by silica gel flash chromatography using a gradient of 80/20 to 20/80 heptane/ethyl acetate providing an orange solid. Yield (3.8 g, 62%). 1H NMR (400 MHz, CDCl3) δ ppm 1.67 (t, J=5.08 Hz, 1H) 3.77-3.83 (m, 2H) 3.88-3.94 (m, 2H) 6.51 (ddd, J=9.77, 8.59, 7.03 Hz, 1H) 8.02 (ddd, J=9.77, 5.66, 2.34 Hz, 1H) 8.21 (s, 1H)

1. concentrationThe reaction is concentrated to dryness
2. custompurified by silica gel flash chromatography
3. customYield (3.8 g, 62%)