Reaktion #46851

Reaktionsgleichung

KMnO4

8-Hydroxymethyl-1,3-dimethyl-3,7-dihydro-purine-2,6-dione

NaOH

→

1,3-Dimethyl-2,6-dioxo-2,3,6,7-tetrahydro-1H-purine-8-carboxylic acid

Lösungsmittel

water

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Filtrationwas filtered over Celite
2. 2
   workup.ADDITIONAfter addition of activated carbon the filtrate
3. 3
   Filtrationwas again filtered over Celite
4. 4
   EinengenThe filtrate was concentrated to a volume of 200 mL and 5 mL of conc. HCl-solution
5. 5
   workup.ADDITIONwere added
6. 6
   workup.WAITAfter standing at 4° C. for 16 h
7. 7
   Filtrationthe crystaline product was filtered off
8. 8
   Waschenwashed twice with cold water and acetone
9. 9
   Sonstigedried under reduced pressure at 40° C.

Vorschrift

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.

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