反应详情

温度

5 °C

A stirred suspension of 6-[2-(2-methoxy-ethoxy)-phenyl]-2-methyl-3H-pyrimidin-4-one (0.17 g, 0.66 mmol) in POCl3 (2 mL) was heated at reflux for 1 h. The reaction mixture was cooled to about 5° C. and poured cautiously into 10 ml ice-water, ammonia (10 mL) was added and extracted with ethyl acetate (2×10 mL), organic layers were combined, washed with water (5 mL) then dried over anhydrous sodium sulfate and concentrated. The residue was purified by column chromatography on silica gel (eluent CHCl3-EtOAc, 10:1), yielding 0.16 g (87%) 4-chloro-6-[2-(2-methoxy-ethoxy)-phenyl]-2-methyl-pyrimidine as colorless solid.

1. temperaturewas heated
2. temperatureat reflux for 1 h
3. additionwas added
4. extractionextracted with ethyl acetate (2×10 mL), organic layers
5. washwashed with water (5 mL)
6. dry with materialthen dried over anhydrous sodium sulfate
7. concentrationconcentrated
8. customThe residue was purified by column chromatography on silica gel (eluent CHCl3-EtOAc, 10:1)