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2,4-Dichloro-5-ethoxy-pyrimidine[0095] In ice bath, dimethyl-phenyl-amine (5.21ml, 1.0 eq) was added dropwise to slurry of 5-ethoxy-pyrimidine-2,4-diol (6.45 g, 1.0 eq) in POCl3 (20 ml, 5.0 eq) and refluxed overnight. Excess POCl3 was evaporated in vacuo and the residue was poured into ice-water. After formation of precipitates, the mixture was filtered and dried solid in vacuo. A product was obtained as a white solid (2.84 g, 35.57percent)1H NMR (500 MHz, CDCl3-di): 51.47-1.50(m, 3H), 4.16-4.20(m, 2H), 8.13(s, 1H)
Method 61 2,4-Dichloro-5-ethoxypyrimidine Using an analogous method to that described in Method 8, but starting from 5-ethoxyuracil (obtained by an analogous method to that described for the preparation of 5-methoxyuracil in J. Chem. Soc., 1960, 4590), the product was obtained in 25% yield. NMR (CDCl3): 1.45 (t, 3H), 4.15 (q, 2H), 8.1 (s, 1H).
-(2-Chloro-5-ethoxy- yrimidin-4-yl)-mo holine [0096] 2,4-dichloro-5-ethoxy-pyrimidin (2.83 g, 1.0 eq) was stirred in toluene(20 ml) and a solution of morpholine (1.93 ml, 1.5 eq) in toluene (20 ml) was added dropwise at -10~0C. After stirring the resulting solution overnight at r.t, NH4Cl(aq) was added to the solution and the solution was extracted with EA. The combined organic layers were washed with brine, dried and evaporated in vacuo. A product was obtained as a white solid (2.7 g , 73.5%).1H NMR (500 MHz, CDCl3-di): 61.41-1.44(m, 3H), 3.75-3.77(m, 4H), 3.83-3.85(m, 4H), 4.01-4.05(m, 2H), 7.69(s, 1H)
With N,N-dimethyl-aniline; trichlorophosphate;Reflux;
2,4-Dichloro-5-ethoxy-pyrimidine[0095] In ice bath, dimethyl-phenyl-amine (5.21ml, 1.0 eq) was added dropwise to slurry of 5-ethoxy-pyrimidine-2,4-diol (6.45 g, 1.0 eq) in POCl3 (20 ml, 5.0 eq) and refluxed overnight. Excess POCl3 was evaporated in vacuo and the residue was poured into ice-water. After formation of precipitates, the mixture was filtered and dried solid in vacuo. A product was obtained as a white solid (2.84 g, 35.57%)1H NMR (500 MHz, CDCl3-di): 51.47-1.50(m, 3H), 4.16-4.20(m, 2H), 8.13(s, 1H)
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