反应详情

温度

70 °C

0.36 g of 4-(2-butynyloxy)-5,6-difluoropyrimidine, 0.25 g of 3,3-dimethylpyrrolidine hydrochloride and 0.62 g of potassium carbonate are added to 1 ml of acetonitrile, then the reaction mixture is stirred at 70° C. for 5 hours. Then saturated aqueous solution of ammonium chloride is added to the reaction mixture which is cooled to about room temperature, and extract with t-butyl methyl ether three times. The organic layers are joined, dried with anhydrous magnesium sulfate, and concentrated. The residue is subjected to silica gel column chromatography to obtain 4-(2-butynyloxy)-5-fluoro-6-(3,3-dimethylpyrrolidine-1-yl)pyrimidine (referred as the present compound (8) hereinafter).

1. temperatureis cooled to about room temperature
2. extractionextract with t-butyl methyl ether three times
3. dry with materialdried with anhydrous magnesium sulfate
4. concentrationconcentrated