反应详情

To a suspension of 0.05g of sodium hydride(purity:60%) and 5 ml of tetrahydrofuran, 0.5g of 3-(4-chloro-2-fluoro-5-methanesulfonylaminophenyl)-1-methyl-6-trifluoromethyl-2,4(1H, 3H)-pyrimidinedione was added at a temperature of 0° C. Then 0.11 ml of methanesulfonyl chloride was added dropwise to the resultant suspension. After stirring for 7 hburs, the reaction mixture was poured into ice water and extracted with ethyl acetate. The extract of the ethyl acetate layer was washed with a saturated sodium chloride agueous solution and dried over anhydrous sodium sulfate. Then ethyl acetate was distilled off to obtain a crude product. The obtained product was washed with diethyl ether to obtain 0.50g of the objective product as white crystals.

1. additionwas added at a temperature of 0° C
2. extractionextracted with ethyl acetate
3. extractionThe extract of the ethyl acetate layer
4. washwas washed with a saturated sodium chloride agueous solution
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThen ethyl acetate was distilled off
7. customto obtain a crude product
8. washThe obtained product was washed with diethyl ether