HRID2104103

反应详情

EQUATION

反应方程式

HRID 2104103 的结构方程式

PROCEDURE

实验过程

3-Phenyl-7H-thieno[2,3-b]pyridine-4-one (0.7 g, 4.29 mmol) was added to phosphorous oxychloride (10 ml) and heated to reflux for 4 hr. The solvent was removed to near dryness and the residue dissolved in DCM. The solution was washed with water followed by saturated sodium hydrogen carbonate and dried over magnesium sulfate. The solution was filtered through a pad of silica and solvents removed in vacuo to give 4-chloro-3-phenyl-thieno[2,3-b]pyridine. Yield=0.261g (25%).

WORKUP

后处理

  1. temperatureheated
  2. temperatureto reflux for 4 hr
  3. customThe solvent was removed
  4. dissolutionthe residue dissolved in DCM
  5. washThe solution was washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationThe solution was filtered through a pad of silica and solvents
  8. customremoved in vacuo