Reaktion #2091

Reaktionsgleichung

benzyl chloride

sodium hydride

3-methylxanthine

hydrogen

→

7-Benzyl-3-methylxanthine

Lösungsmittel

water

dimethylformamide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated at 120° C. for a further 6 hours
2. 2
   TemperaturThe reaction mixture was cooled
3. 3
   FiltrationThe solid was filtered off with suction
4. 4
   Waschenwashed with water
5. 5
   FiltrationThe crystallizate was filtered
6. 6
   Waschenwashed with ethanol
7. 7
   Sonstigedried under reduced pressure

Vorschrift

16.8 g (0.7 mol) of sodium hydride were introduced in portions with stirring into a suspension of 99.6 g (0.6 mol) of 3-methylxanthine in 1.5 l of dimethylformamide. After evolution of hydrogen had ended, the mixture was heated to 100° C., treated dropwise with 76 g (0.6 mol) of benzyl chloride and heated at 120° C. for a further 6 hours. The reaction mixture was cooled and cautiously poured into 3 l of water. The solid was filtered off with suction and washed with water, the filter residue was taken up in ethanol and the solution was stirred at room temperature for one hour. The crystallizate was filtered, washed with ethanol and dried under reduced pressure.

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