反应详情

1.00 g (2.41 mmol) of 3-(4-chloro-5-ethylsulfonylamino-2-fluorophenyl)-6-trifluoromethyl-2,4(1H,3H)-pyrimidinedione was dissolved in 10 ml of acetone, and 0.17 g (1.20 mmol) of anhydrous potassium carbonate and 0.23 ml (2.41 mmol) of dimethyl sulfate were added thereto and the reaction was continued for 1.5 hours. After acetone was distilled off, the reaction product was dissolved in ethyl acetate, washed with water and saturated saline solution, and dried over anhydrous sodium sulfate. Thereafter the ethyl acetate was distilled off to obtain a crude product. The crude product was recrystallized from chloroformdiethyl ether, thereby obtaining 0.61 g of the objective product (yield: 59%) in the form of light yellow crystals.

1. distillationAfter acetone was distilled off
2. dissolutionthe reaction product was dissolved in ethyl acetate
3. washwashed with water and saturated saline solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThereafter the ethyl acetate was distilled off
6. customto obtain a crude product
7. customThe crude product was recrystallized from chloroformdiethyl ether