HRID12738
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 5-(2-fluoro-6-methyl-pyridin-3-yl)-1H-pyrimidine-2,4-dione hydrochloride (Prep 15, 667 mg, 2.59 mmol), and K2CO3 (358 mg, 2.59 mmol) in DMF (25 ml) was stirred 30 minutes at room temperature. Then 90% 3-Bromo-1,1dimethoxy-propane (432 μl, 2.85 mmol) was added in three portions during 3 days. Solvent was then removed under vacuum at 40° C. and the residue washed with ethyl acetate. The organic 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 291 mg of the title compound as a white solid (35% yield).
WORKUP
后处理
- customSolvent was then removed under vacuum at 40° C.
- washthe residue washed with ethyl acetate
- dry with materialThe organic phase was dried (Na2SO4)
- filtrationfiltered
- customevaporated
- customThe crude was purified by flash chromatography
- washeluting with DCM-MeOH—NH4OH (98-2-0.2)