反应详情

To 2-(4-bromophenyl)-5-(2-chloro-6-fluorophenyl)-2,4-dihydro-3H-1,2,4-triazol-3-one (Intermediate-1, 0.100 g, 0.271 mmol) was added POCl3. The reaction mass was refluxed for 48 h. The reaction mass was quenched in water, basified with NaHCO3 and extracted with ethyl acetate and concentrated. The obtained crude product was purified with column chromatography on silica gel eluting with 0.5% EA:DCM to afford 0.110 g of the desired product. 1H NMR (300 MHz, DMSO d6): δ 7.44 (t, J=9.3 Hz, 1H), 7.53 (d, J=7.8 Hz, 1H), 7.60-7.68 (m, 1H), 7.72 (d, J=9.0 Hz, 2H), 7.85 (d, J=8.7 Hz, 2H). MS (m/z): 388.22 (M+H)+.

1. temperatureThe reaction mass was refluxed for 48 h
2. customThe reaction mass was quenched in water
3. extractionextracted with ethyl acetate
4. concentrationconcentrated
5. customThe obtained crude product
6. customwas purified with column chromatography on silica gel eluting with 0.5% EA