Reaktion #10007

Reaktionsgleichung

DMF

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

caesium carbonate

iodoethane

→

2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine

Lösungsmittel

ethyl acetate

dioxane water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Waschenthe organic phase is washed with water
2. 2
   Trocknendried over sodium sulfate
3. 3
   SonstigeAfter removal of the solvent
4. 4
   Sonstigethe residue is chromatographed over silica gel (mobile phase: ethyl acetate/hexane=4:1)

Vorschrift

1 g (3.47 mmol) of 2-chloro-6-(3-fluoro-phenyl-amino)-purine, 1.8 g (5.5 mmol) of caesium carbonate and 2.3 ml (27.8 mmol) of iodoethane are stirred in 14 ml of a dioxane/water mixture (4:3) and 12 ml of DMF at RT for 16 h. Thereafter, the reaction mixture is diluted with ethyl acetate and the organic phase is washed with water and dried over sodium sulfate. After removal of the solvent, the residue is chromatographed over silica gel (mobile phase: ethyl acetate/hexane=4:1) and 2-chloro-9-ethyl-6-(3-fluoro-phenyl-amino)-9H-purine is isolated; m.p. 136° C.; FAB-MS: (M+H)+=292; Rf=0.7 (CH2Cl2:methanol=9:1).

Quelle