反应详情

温度

5 °C

5.00 g (24.0 mmol) 8-Hydroxymethyl-1,3-dimethyl-3,7-dihydro-purine-2,6-dione were suspended in 15 mL water. 16.8 mL (33.6 mmol) of a 2 N NaOH-solution were added. The resulting mixture was cooled to 5° C. At that temperature a solution of 5.05 g (32.2 mmol) KMnO4 in 86 mL water was added. After stirring at room temperature for 4 h the reaction mixture was filtered over Celite. After addition of activated carbon the filtrate was again filtered over Celite. The filtrate was concentrated to a volume of 200 mL and 5 mL of conc. HCl-solution were added. After standing at 4° C. for 16 h the crystaline product was filtered off, washed twice with cold water and acetone and dried under reduced pressure at 40° C.

1. filtrationwas filtered over Celite
2. additionAfter addition of activated carbon the filtrate
3. filtrationwas again filtered over Celite
4. concentrationThe filtrate was concentrated to a volume of 200 mL and 5 mL of conc. HCl-solution
5. additionwere added
6. waitAfter standing at 4° C. for 16 h
7. filtrationthe crystaline product was filtered off
8. washwashed twice with cold water and acetone
9. customdried under reduced pressure at 40° C.