HRID420681
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
4-(2,2-Dimethyl-1,3-dioxan-5-yl)-6-(methyloxy)-1,4-dihydropyrido[2,3-b]pyrazin-3(2H)-one (25.37 g) and activated manganese dioxide (120 g) were stirred in DCM (500 ml) at room temperature for 2 h. The mixture was filtered with suction and the solids were washed with DCM (2×100 ml). The combined filtrate plus washings were evaporated under reduced pressure to give a brown foam; this was purified by column chromatography on silica (eluting with 0%-100% EtOAc in petroleum ether (40-60°)). Appropriate fractions were combined and evaporated under reduced pressure to give the title compound as a light tan solid (17.40 g, 69%).
WORKUP
后处理
- filtrationThe mixture was filtered with suction
- washthe solids were washed with DCM (2×100 ml)
- customThe combined filtrate plus washings were evaporated under reduced pressure
- customto give a brown foam
- customthis was purified by column chromatography on silica (eluting with 0%-100% EtOAc in petroleum ether (40-60°))
- customevaporated under reduced pressure