反应详情

温度

5 °C

45.9 Grams of 2,4,6-trichloro-5-methylthio-pyrimidine, 150 g of methylethylketone and 130 g of water are introduced into a 250 ml reactor provided with a stirrer. To this mixture maintained at 5° C. are added in a period of 30 minutes 9.44 g of ethylamine in 32.5% aqueous solution. The temperature of 5° C. is maintained for one and one half hours. Then 8.08 g of caustic soda in 30% aqueous solution are added. The mixture is maintained at 20° C. for 4 hours and over night in a refrigerator at about 0° C. A precipitate appears which is isolated by filtration, washed with 16 ml of methylethylketone and recrystallized twice from 180 ml of ethanol. 10.5 G of 2-ethylamino-4,6-dichloro-5-methylthio-pyrimidine are thus obtained, which melts at 147° C. and which is identified by its infra-red spectrum (IR) and it nuclear magnetic resonance spectrum (NMR).

1. customprovided with a stirrer
2. temperatureThe temperature of 5° C. is maintained for one and one half hours
3. temperatureThe mixture is maintained at 20° C. for 4 hours and over night in a refrigerator at about 0° C
4. customis isolated by filtration
5. washwashed with 16 ml of methylethylketone
6. customrecrystallized twice from 180 ml of ethanol