反应详情

温度

35 °C

19.92 g (0.1 mole) of 2-amino-4-(2-hydroxyethylamino)-5-nitropyrimidine was suspended in 400 ml of methanol, to which 10 g of wet Raney nickel was then added. The mixture was stirred at a temperature of 30-40° C. for 3 hours. After completion of the reaction, the reaction product was filtered through nitrocellulose, followed by washing. The filtrate was concentrated under reduced pressure. To the remaining concentrate, 100 ml of triethylorthoformate and 10 ml of concentrated hydrochloric acid were added, and the mixture was stirred under reflux for 9 hours at a temperature of 80-90° C. After completion of the reaction, the product was cooled to room temperature, and 200 ml of ethylether was then added thereto. The resulting crystal was filtered, washed and dried, thereby giving 13.44 g (75% yield) of yellowish brown-colored 2-amino-9-(2-hydroxyethyl)purine.

1. additionwas then added
2. customAfter completion of the reaction
3. filtrationthe reaction product was filtered through nitrocellulose
4. washby washing
5. concentrationThe filtrate was concentrated under reduced pressure
6. concentrationTo the remaining concentrate
7. addition100 ml of triethylorthoformate and 10 ml of concentrated hydrochloric acid were added
8. stirringthe mixture was stirred
9. temperatureunder reflux for 9 hours at a temperature of 80-90° C
10. customAfter completion of the reaction
11. temperaturethe product was cooled to room temperature
12. filtrationThe resulting crystal was filtered
13. washwashed
14. customdried