反应详情

温度

90 °C

To a suspension of 18.93 g (80 mmol) of 3-benzyl-6-chloropyrimidine-2,4(1H,3H)-dione and 17.69 g (128 mmol) of potassium carbonate in 120 ml of N,N-dimethylformamide, 15.8 ml (160 mmol) of 1-bromo-3-chloropropane was added at room temperature. This mixture was stirred at 90° C. for 3 hours. After cooling, the reaction mixture was concentrated to dryness; the resulting residue was dissolved in chloroform-water. After the organic layer was washed with water and dried, the solvent was distilled off to yield an oily substance, which was then purified by column chromatography (eluent, n-hexane/ethyl acetate=5/1→3/1) to yield 13.46 g (53.7%, light yellow powder) of the desired product.

1. additionwas added at room temperature
2. temperatureAfter cooling
3. concentrationthe reaction mixture was concentrated to dryness
4. dissolutionthe resulting residue was dissolved in chloroform-water
5. washAfter the organic layer was washed with water
6. customdried
7. distillationthe solvent was distilled off
8. customto yield an oily substance, which
9. customwas then purified by column chromatography (eluent, n-hexane/ethyl acetate=5/1→3/1)