Reaktion #9998

Reaktionsgleichung

2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine

caesium carbonate

ethyl iodide

→

2-Chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine

Lösungsmittel

dioxane water DMF

ethyl acetate

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenthe organic phase is washed with water
2. 2
   SonstigeThis phase is separated off
3. 3
   Trocknendried over sodium sulfate
4. 4
   SonstigeAfter removal of the solvent
5. 5
   Sonstigethe residue is recrystallized from ethyl acetate and diethyl ether

Vorschrift

A mixture comprising 1 g (3.2 mmol) of 2-chloro-6-(3-trifluoromethyl-phenyl-amino)-purine, 1.7 g (5.1 mmol) of caesium carbonate and 2.1 ml (25.6 mmol) of ethyl iodide in 7 ml of dioxane/water/DMF (8:2:2) is stirred at RT for 18 h. It is then diluted with ethyl acetate and the organic phase is washed with water. This phase is separated off and dried over sodium sulfate. After removal of the solvent, the residue is recrystallized from ethyl acetate and diethyl ether. 2-Chloro-9-ethyl-6-(3-trifluoromethyl-phenyl-amino)-9H-purine is obtained; m.p. 129–130° C.; FAB-MS: (M+H)+=342; Rf=0.6 (methylene chloride:methanol=9:1).

Quelle