HRID453117

反应详情

EQUATION

反应方程式

HRID 453117 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

To a solution of 4-chloro-2-hydroxybenzamide (0.608 g, 3.54 mmol) in acetonitrile (50 ml) was added dried K2CO3 (1.71 g, 12.40 mmol) followed by benzyl bromide (0.63 ml, 5.32 mmol) and the resulting reaction mixture was refluxed at 80° C. for 16 h. After the completion of the reaction (TLC monitoring), water was added followed by extraction with EtOAc (3×100 ml). The combined organics was dried over anhydrous Na2SO4, filtered and concentrated. The residue was washed repeatedly with hexane to get rid of the excess of benzyl bromide resulting the desired product (0.75 g, 81%).

WORKUP

后处理

  1. customthe resulting reaction mixture
  2. additionwas added
  3. extractionfollowed by extraction with EtOAc (3×100 ml)
  4. dry with materialThe combined organics was dried over anhydrous Na2SO4
  5. filtrationfiltered
  6. concentrationconcentrated
  7. washThe residue was washed repeatedly with hexane