HRID7604
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- customThe excess phosphorus oxychloride is evaporated in vacuo
- additionthe residue is poured, on ice cold aqueous NaHCO3
- extractionextracted with ethyl acetate
- washThe organic layer is washed with brine
- customdried
- filtrationfiltered
- customevaporated
- customThe resulting residue is purified on flash chromatography (SiO2, hexane/AcOEt gradient)