HRID2210788

反应详情

EQUATION

反应方程式

HRID 2210788 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of methyl (E)-3-[2-(4-imidazolylmethylamino)phenyl]propenoate (0.7 g) in methanol (7 ml) was added 1N sodium hydroxide aqueous solution (3 ml) and the mixture was stirred for 20 hours. After removal of methanol from the reaction mixture, water was added to the residue. The mixture was adjusted to pH 6 with acetic acid. The mixture was salted out and extracted with ethyl acetate 8 times. The extracts were combined and dried over magenessium sulfate. Removal of the solvent afforded an orange oil, which was dissolved in methanol (5 ml). To the solution was added an ethereal solution of hydrogen chloride. The resultant precipitate was collected by filtration, washed with ether twice and dried to give (E)-3-[2-(4-imidazolylmethylamino)phenyl]propenoic acid dihydrochloride (0.29 g).

WORKUP

后处理

  1. customAfter removal of methanol from the reaction mixture, water
  2. additionwas added to the residue
  3. extractionextracted with ethyl acetate 8 times
  4. dry with materialdried over magenessium sulfate
  5. customRemoval of the solvent
  6. customafforded an orange oil, which
  7. filtrationThe resultant precipitate was collected by filtration
  8. washwashed with ether twice
  9. customdried