HRID7604

反应详情

EQUATION

反应方程式

HRID 7604 的结构方程式

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

To a solution of 4-hydroxy-2-phenoxymethylquinazoline (2 g, 7.93 mmol) in phosphorus oxychloride (10 mL) is added tripropylamine (3.02 mL, 15.8 mmol) and the reaction mixture is heated for 30 minutes at 110° C. The excess phosphorus oxychloride is evaporated in vacuo, the residue is poured, on ice cold aqueous NaHCO3 and extracted with ethyl acetate. The organic layer is washed with brine, dried, filtered and evaporated. The resulting residue is purified on flash chromatography (SiO2, hexane/AcOEt gradient) to give 4-chloro-2-phenoxymethylquinazoline.

WORKUP

后处理

  1. customThe excess phosphorus oxychloride is evaporated in vacuo
  2. additionthe residue is poured, on ice cold aqueous NaHCO3
  3. extractionextracted with ethyl acetate
  4. washThe organic layer is washed with brine
  5. customdried
  6. filtrationfiltered
  7. customevaporated
  8. customThe resulting residue is purified on flash chromatography (SiO2, hexane/AcOEt gradient)