preparation | in a ML round-bottom flask, 4-chloro-6-methylpyrimidin-2-amine (3G, 21.0mmol) was dissolved in 40ml glacial acetic acid and cooled to below 10 °c in an ice bath. NIS(2.4g,10.6mmol) was added to the upper solution, and after reacting for 1 hour, NIS(2.4g,10.6mmol) was added again, and after reacting for 1 hour, it was naturally raised to room temperature and reacted for 8 hours. After completion of the reaction, the reaction solution was poured into ice water and extracted with EtOAc. The organic phase was washed with 5%Na2SO3 solution, 10% NaHCO3 solution and saturated NaCl solution, and dried over anhydrous Na2SO4, after filtration, the solvent was removed by concentration under reduced pressure to obtain 87% G of a solid, that is, 2-amino-4-chloro-6-methylpyrimidin-5-carbonitrile. |