Diethyl Ether → 2-(2-Aminopurin-9-yl)ethanol

Temperature

35 °C

19.92 g (0.1 mole) of 2-amino-4-(2-hydroxyethylamino)-5-nitropyrimidine was suspended in 400 ml of acetic acid, to which 20 g of iron powder 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 resulting 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 crude product was cooled to room temperature, and 200 ml of ethylether was added thereto. The resulting crystal was filtered, washed and dried, thereby giving 10.75 g (60% 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 resulting 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. filtrationThe resulting crystal was filtered
12. washwashed
13. customdried

ORD record

ord-76c134df36964c8bbce62f504fe23b57

Source dataset

uspto-grants-2008_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07456282B2