反应详情

To a suspension of 5-(2-chloro-pyridin-3-yl)-1H-pyrimidine-2,4-dione hydrochloride salt (Prep95, 803 mg, 3.10 mmol) and K2CO3 (428 mg, 3.10 mmol) in DMF (15 ml), 90% 3-bromo-1,1dimethoxy-propane (516 μl, 3.41 mmol) was added in three portions over 5 days. The mixture was contemporarily stirred at room temperature. Solvent was then removed in vacuum at 40° C. The residue washed with petroleum ether and then with ethyl acetate. Ethyl acetate phase was dried (Na2SO4), filtered and evaporated. The crude was purified by flash chromatography eluting with DCM-MeOH—NH4OH (98:2:0.2) to give 400 mg of the final compound as a white solid (40% yield)

1. additionwas added in three portions over 5 days
2. customSolvent was then removed in vacuum at 40° C
3. washThe residue washed with petroleum ether
4. dry with materialEthyl acetate phase was dried (Na2SO4)
5. filtrationfiltered
6. customevaporated
7. customThe crude was purified by flash chromatography
8. washeluting with DCM-MeOH—NH4OH (98:2:0.2)