反应详情

A mixture of 3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione(4.5 g, 0.01 mol), phosphorus oxychloride(1.5 g, 0.01 mol), triethylamine(2.0 g, 0.02 mol) and toluene(14 ml) was heated under reflux for 24 hours. The reaction mixture was poured into water and extracted with ethyl acetate. The ethyl acetate solution contained 3.5 g(yield 76%) of the above compound III-1(HPLC analysis). The ethyl acetate solution was concentrated and purified by column chromatography on silica gel(20% ethyl acetate/hexane) to give compound III-1 as a white solid, m.p.128-131° C.

1. temperaturewas heated
2. temperatureunder reflux for 24 hours
3. extractionextracted with ethyl acetate