反应详情

To a mixture of 1.00 g of 3-(5-amino-4-chloro-2-fluorophenyl)-1-methyl-6-trifluoromethyl-2,4 (1H,3H)-pyrimidinedione, 0.63 g of triethylamine and 10 ml of dichloromethane, 0.48 g of methanesulfonylchloride was added at a temperature of not more than 5° C. The resultant mixture was stirred overnight. After washing twice the reaction mixture with water, the reaction mixture was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The dichloromethane was distilled off to obtain a crude product. The obtained product was washed with diisopropylether to obtain 1.36 g of the objective product as white crystals. m.p.: 282°~285° C.

1. additionwas added at a temperature of not more than 5° C
2. washAfter washing twice the reaction mixture with water
3. washthe reaction mixture was washed with a saturated sodium chloride aqueous solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe dichloromethane was distilled off
6. customto obtain a crude product
7. washThe obtained product was washed with diisopropylether