反应详情

温度

5 °C

A stirred suspension of 6-[2-(2-methoxy-ethoxy)-phenyl]-3H-pyrimidin-4-one (0.2 g, 0.81 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 triturated with hexane yielding 0.18 g (84%) 4-chloro-6-[2-(2-methoxy-ethoxy)-phenyl]-pyrimidine as white powder.

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 triturated with hexane yielding 0.18 g (84%) 4-chloro-6-[2-(2-methoxy-ethoxy)-phenyl]-pyrimidine as white powder