HRID1710690

反应详情

EQUATION

反应方程式

HRID 1710690 的结构方程式

PROCEDURE

实验过程

A suspension of 5-(3-fluoropyridin-4-yl)-6-pyridin-3-ylpyrazin-2(1H)-one (0.79 g, 2.95 mmol) in phosphorus oxychloride (5 mL) was heated to reflux and stirred overnight. The mixture was evaporated and carefully neutralised with 4% aqueous sodium hydrogen carbonate solution with external cooling. The mixture was extracted with ethyl acetate and the organic layer was washed with brine, dried (MgSO4) and evaporated. The residue was purified by silica gel chromatography (CH2Cl2 to CH2Cl2/MeOH 98:2) to give the title compound (0.279 g, 33%) as an off-white solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux
  3. customThe mixture was evaporated
  4. extractionThe mixture was extracted with ethyl acetate
  5. washthe organic layer was washed with brine
  6. dry with materialdried (MgSO4)
  7. customevaporated
  8. customThe residue was purified by silica gel chromatography (CH2Cl2 to CH2Cl2/MeOH 98:2)