反应详情

温度

60 °C

16.8 g (0,040 mol) of methyl 4-(4-chlorophenyl)-2-(4,6-dimethoxypyrimidin-2-ylthio)nicotinate was dissolved in 150 ml of dimethylsulfoxide, and 35 ml (0,070 mol) of 2N sodium hydroxide added with stirring at 60° C. After stirring at 60° C. for 30 minutes, the mixture was poured into water, and washed twice with ethyl acetate. The aqueous layer was acidified with 10% hydrochloric acid, and extracted with 500 ml of ethyl acetate. The extract was washed with water and a saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate, and concentrated. The concentrate was washed with methanol and isopropyl ether to obtain 11.5 g of a white crystal of the aimed product.

1. stirringAfter stirring at 60° C. for 30 minutes
2. washwashed twice with ethyl acetate
3. extractionextracted with 500 ml of ethyl acetate
4. washThe extract was washed with water
5. dry with materiala saturated aqueous solution of sodium chloride, and dried over anhydrous sodium sulfate
6. concentrationconcentrated
7. washThe concentrate was washed with methanol and isopropyl ether