反应详情

50 ml of POCl3 was added dropwise to a solution of 14.5 g (0.1 mol) of 4-hydroxyl-5-chloro-6-methylpyrimidine in 50 mL of toluene, the mixture was refluxed for 5-7 h after addition. After the reaction was over by Thin-Layer Chromatography monitoring, the reaction mixture was concentrated under reduced pressure to remove toluene and extra POCl3, and then poured into ice water. The water phase was extracted with ethyl acetate (3×50 ml), the organic phases were emerged, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was purified through silica column to give 14.43 g as yellow liquid with yield of 88.5%.

1. temperaturethe mixture was refluxed for 5-7 h
2. additionafter addition
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customto remove toluene and extra POCl3
5. additionpoured into ice water
6. extractionThe water phase was extracted with ethyl acetate (3×50 ml)
7. dry with materialdried over anhydrous magnesium sulfate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure
10. customThe residue was purified through silica column
11. customto give 14.43 g as yellow liquid with yield of 88.5%