反应详情

温度

70 °C

22.6 g (70.5 mmol) of 3-(4-chloro-2-hydroxyphenyl-1-methyl-6-trifluoromethyluracil and 14.5 g (105.1 mmol) of potassium carbonate were suspended in 150 ml of N,N-dimethylformamide, and 11.2 g (94.1 mmol) of propargyl bromide was dropwise added thereto at room temperature. After stirring at 70° C. for 2 hours, the reaction solution was poured into water and extracted with ethyl acetate. The organic layer was washed sequentially with water and a saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure. Then, the obtained crude crystals were washed with isopropyl ether to obtain 22.5 g (yield: 89.0%) of the desired product as pale brown powder. Melting point: 147-148° C.

1. customat room temperature
2. extractionextracted with ethyl acetate
3. washThe organic layer was washed sequentially with water
4. dry with materiala saturated sodium chloride aqueous solution and then, dried over anhydrous magnesium sulfate
5. distillationThe solvent was distilled off under reduced pressure
6. customThen, the obtained crude crystals
7. washwere washed with isopropyl ether