HRID424356

反应详情

EQUATION

反应方程式

HRID 424356 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)-2-(5-((2,4,6-trimethoxystyrylsulfonyl)methyl)-2-methoxyphenylamino)propanoate (0.1 mol) in ethanol (200 mL), was added sodium hydroxide (20% aqueous solution, 200 mL). The resulting mixture was heated at reflux for 2.5 h. The reaction was monitored by TLC. When the reaction was complete, the volatiles were removed under vacuum and the resulting residue was acidified to pH 4 by addition of acetic acid. A solid precipitate formed. The precipitate was separated by filtration. The filtered solid was recrystallized twice from acetone to provide the desired (E)-2-(5-((2,4,6-trimethoxystyrylsulfonyl)methyl)-2-methoxyphenylamino)propanoic acid. m.p. 176-180° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux for 2.5 h
  3. customthe volatiles were removed under vacuum
  4. additionthe resulting residue was acidified to pH 4 by addition of acetic acid
  5. customA solid precipitate formed
  6. customThe precipitate was separated by filtration
  7. customThe filtered solid was recrystallized twice from acetone