反应详情

A mixture of 2-chloro-3-[4-chloro-2-fluoro-5-(2-nitrophenoxy)phenyl]-6-trifluoromethyl-4(3H)-pyrimidinone(1.28 g, 0.0027 mol), cyclopentanone oxime(027 g, 0.0027 mol), potassium carbonate(0.38 g, 0.027 mol) and tetrahydrofuran(11 ml) was heated under reflux for 3 hours. The reaction mixture was poured into water, extracted with ethyl acetate, and washed with brine. The organic phase was dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography on silica gel(20% ethyl acetate/hexane) to give compound II-3 (1.23 g, yield 84.7%) as a white amorphous solid, m.p.76-78° C.

1. temperaturewas heated
2. temperatureunder reflux for 3 hours
3. extractionextracted with ethyl acetate
4. washwashed with brine
5. dry with materialThe organic phase was dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. customThe residue was purified by column chromatography on silica gel(20% ethyl acetate/hexane)
8. customto give compound II-3 (1.23 g, yield 84.7%) as a white amorphous solid, m.p.76-78° C.