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0 °C

To a solution of 0.112 g (0.48 mmol) of (+/−) 2-(1-amino-ethyl)-1-methyl-1H-[4,4′]bipyrimidinyl-6-one in 5 mL of dimethylformamide was added 0.082 g (0.48 mmol) of 4-fluoro-2-methoxy-benzoic acid and 90 μL (0.58 mmol) of diethyl phosphorocyanidate (DEPC). The resulting mixture was cooled at 0° C., 70 μL (0.53 mmol) of triethylamine was added and stirred at room temperature for 1 h. Water was added and the mixture extracted with diethyl acetate. The extracts were washed with a saturated aqueous solution of ammonium chloride, dried and evaporated. The residue was purified on preparative thin layer chromatography eluting with a mixture of dichloromethane/methanol/aqueous ammonia solution (29%) in the proportions 95/5/0.5 to afford 0.12 g (66%) of the desired compound as a white powder.

1. extractionthe mixture extracted with diethyl acetate
2. washThe extracts were washed with a saturated aqueous solution of ammonium chloride
3. customdried
4. customevaporated
5. customThe residue was purified on preparative thin layer chromatography
6. washeluting with a mixture of dichloromethane/methanol/aqueous ammonia solution (29%) in the proportions 95/5/0.5