反应详情

温度

70 °C

To a suspension of 5.6 g of (2S)-7-hydroxy-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one in 100 mL of 1,2-dichloroethane, are added at room temperature and under an argon atmosphere, 11 mL of phosphorus oxychloride. The resulting mixture is then heated to 70° C. After two hours of stirring and after monitoring with LC/MS, the reaction is completed. After cooling, the reaction mixture is dry evaporated under reduced pressure. The obtained residue is taken up with 5 mL of cold water and 200 mL of ethyl acetate. On the obtained mixture, 32% soda is added up to a pH=6. The organic phase is then separated and then dried on magnesium sulphate, filtered and concentrated under reduced pressure in order to obtain 6 g of (2S)-7-chloro-2-methyl-2-(trifluoromethyl)-2,3-dihydroimidazo[1,2-a]pyrimidin-5(1H)-one including the following characteristics:

1. additionare added at room temperature and under an argon atmosphere
2. temperatureAfter cooling
3. customthe reaction mixture is dry
4. customevaporated under reduced pressure
5. additionOn the obtained mixture, 32% soda is added up to a pH=6
6. customThe organic phase is then separated
7. customdried on magnesium sulphate
8. filtrationfiltered
9. concentrationconcentrated under reduced pressure in order