Reaktion #2148

Reaktionsgleichung

sodium hydride

3-phenylxanthine

benzyl bromide

→

7-Benzyl-3-phenylxanthine

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated to 80° C
2. 2
   workup.WAITthe solution was left at 80° C. for 6 hours
3. 3
   TemperaturAfter cooling to 50° C.
4. 4
   Sonstigethe precipitate obtained
5. 5
   Filtrationwas filtered off with suction
6. 6
   Waschenwashed well with water
7. 7
   Sonstigedried under reduced pressure
8. 8
   SonstigeThe dry residue was crystallized from dioxane/methanol

Vorschrift

3.2 g (0.1315 mol) of sodium hydride were added in portions to a suspension of 30 g (0.1315 mol) of 3-phenylxanthine in 600 ml of DMF, the mixture was stirred at 25° C. for 30 minutes and then heated to 80° C. 27 g (0.1578 mol) of benzyl bromide were then added and the solution was left at 80° C. for 6 hours. After cooling to 50° C., the reaction mixture was poured into 2000 ml of ice-water, and the precipitate obtained was filtered off with suction, washed well with water and dried under reduced pressure. The dry residue was crystallized from dioxane/methanol.

Quelle