HRID1943193

反应详情

EQUATION

反应方程式

HRID 1943193 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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, ˜15 eq.) were stirred in DCM (500 ml) at room temperature for 2 hours then overnight. 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% ethyl acetate 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

  1. customovernight
  2. filtrationThe mixture was filtered with suction
  3. washthe solids were washed with DCM (2×100 ml)
  4. customThe combined filtrate plus washings were evaporated under reduced pressure
  5. customto give a brown foam
  6. customthis was purified by column chromatography on silica (eluting with 0%-100% ethyl acetate in petroleum ether (40-60°))
  7. customevaporated under reduced pressure