HRID606820

反应详情

EQUATION

反应方程式

HRID 606820 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Heat a solution of 5-bromo-2-fluorobenzoic acid (20 g, 92 mmol) and p-toluenesulfonic acid monohydrate (52 g, 275 mmol) in methanol (200 mL) at reflux overnight. Concentrate and dissolve the residue in ethyl acetate, wash twice with an aqueous saturated solution of sodium bicarbonate, once with an aqueous saturated solution of sodium chloride, dry (sodium sulfate), filter and concentrate to give the title compound as a clear liquid (19.7 g, 92%).

WORKUP

后处理

  1. temperatureat reflux overnight
  2. concentrationConcentrate
  3. dissolutiondissolve the residue in ethyl acetate
  4. washwash twice with an aqueous saturated solution of sodium bicarbonate, once with an aqueous saturated solution of sodium chloride
  5. dry with materialdry (sodium sulfate)
  6. filtrationfilter
  7. concentrationconcentrate