反应详情

3-[2-(2,4-Dichlorophenyl)ethyl]-7-nitro-2,4(1H, 3H)-quinazolinedione (2.0 g, 5.26 mmol) and PCl5 (1.2 g, 5.79 mmol) were added to a flask containing POCl3 (20 mL) and the resulting solution was refluxed with stirring for 6 hours. The reaction was allowed to cool to RT and stirred overnight at this temp. The POCl3 was removed under reduced pressure and CH2Cl2 was added to the residue. The unreacted starting material was removed via vacuum filtration and the product was purified by silica gel flash chromatography (100% CH2Cl2 eluent) to give the product (0.96 g, 46% yield) as a white solid. 1H NMR (DMSO-D6) 400 MHz δ ppm 8.35-8.25 (m, 3H), 7.58 (d, J=2.2 Hz, 1H), 7.41-7.34 (m, 2H), 4.41 (t, J=7.5 Hz, 2H), 3.15 (t, J=7.5 Hz, 2H) ppm.

1. temperaturethe resulting solution was refluxed
2. stirringstirred overnight at this temp
3. customThe POCl3 was removed under reduced pressure and CH2Cl2
4. additionwas added to the residue
5. customwas removed via vacuum filtration
6. customthe product was purified by silica gel flash chromatography (100% CH2Cl2 eluent)