反应详情

温度

65 °C

To a solution of 6-chloro-3-methyluracil (1 equiv., 1 wt.), N-methylpyrrolidone (NMP; 4 vol.) and diisopropylethylamine (Hünig's base, 1.5 equiv., 1.21 wt.), was added a solution of α-bromotoluoylnitrile (1.1 equiv., 1.35 wt.) and toluene (4 vol.). The mixture was heated at 60-70° C. and agitated for 2-3 hrs, or until completion. The solution was then cooled to 20-30° C., quenched with deionized water (5 vol.) at less than 35° C., agitated for 30 min, cooled to 0-5° C., and then agitated for at least one hour. The resultant slurry was filtered, reslurried in isopropanol, displacement washed with isopropanol, and dried under vacuum at 55-60° C.

1. temperatureThe solution was then cooled to 20-30° C.
2. customquenched with deionized water (5 vol.) at less than 35° C.
3. stirringagitated for 30 min
4. temperaturecooled to 0-5° C.
5. stirringagitated for at least one hour
6. filtrationThe resultant slurry was filtered
7. washdisplacement washed with isopropanol
8. customdried under vacuum at 55-60° C.