HRID725885

反应详情

EQUATION

反应方程式

HRID 725885 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

[2-(2-Chloro-6-methoxyquinolin-4-yl)ethenyl]dimethylamine (28.3 g, 0.11 mol) and hydroxylamine-O-sulfonic acid (40.2 g, 0.36 mol) were suspended in water (1.2 L), and the mixture was stirred at room temperature for 70 hours. The reaction mixture was neutralized with an aqueous solution of sodium hydroxide, and the organic materials were extracted with a mixed solvent of 5% methanol/ethyl acetate. The extract was washed with saturated brine and water and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The resulting residue was recrystallized from ethyl acetate to obtain the title compound (19.9 g, 79%).

WORKUP

后处理

  1. extractionthe organic materials were extracted with a mixed solvent of 5% methanol/ethyl acetate
  2. washThe extract was washed with saturated brine and water
  3. dry with materialdried over anhydrous magnesium sulfate
  4. customThe solvent was evaporated under reduced pressure
  5. customThe resulting residue was recrystallized from ethyl acetate