HRID880697

反应详情

EQUATION

反应方程式

HRID 880697 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To an ice-water cooled solution of 2-methoxy-6-methylaniline (10 g, 72.9 mmol) in 30 mL of methanol and 10 mL of acetic acid was added dropwise bromine (3.75 mL, 72.9 mmol). The reaction mixture was allowed to stand for overnight. The solvent was removed under reduced pressure and the residue was suspended in 60 mL of IN NaOH and extracted with ethyl acetate and dried over sodium sulfate and evaporated to dryness to give reddish crude product, which was recrystallized from hexane to give pure product (14.3 g, 91%).

WORKUP

后处理

  1. customThe solvent was removed under reduced pressure
  2. extractionextracted with ethyl acetate
  3. dry with materialdried over sodium sulfate
  4. customevaporated to dryness
  5. customto give reddish crude product, which
  6. customwas recrystallized from hexane