反应详情

温度

25 °C

To a suspension of 53.7 g of 2-amino-4-cyclopropyl-6-methylpyrimidine in 1000 ml of tetrahydrofuran is added portionwise, under a nitrogen atmosphere, 42.8 g of 50% sodium hydride while cooling the reaction flask in an ice-water bath. After stirring one hour at 25° C. 58.5 g of dimethylcarbonate is added dropwise at 5° to 25°. The suspension is stirred about 16 hours at ambient temperatures, then 80 ml of concentrated hydrocloride acid is added dropwise under a nitrogen atmosphere while maintaining a reaction temperature of 20° to 25° with external ice-bath cooling. The suspension is stirred 0.5 hour, filtered, and the filtrate is dried over sodium sulfate and concentrated in vacuo to give the subject compound.

1. additionis added portionwise, under a nitrogen atmosphere
2. stirringThe suspension is stirred about 16 hours at ambient temperatures
3. temperaturewhile maintaining a reaction temperature of 20° to 25° with external ice-bath
4. temperaturecooling
5. stirringThe suspension is stirred 0.5 hour
6. filtrationfiltered
7. dry with materialthe filtrate is dried over sodium sulfate
8. concentrationconcentrated in vacuo
9. customto give the subject compound