HRID1455723

反应详情

EQUATION

反应方程式

HRID 1455723 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
50 °C

PROCEDURE

实验过程

A solution of N-(4-methoxy-3-nitrophenyl)-3-(2,4,6-trimethoxyphenyl) -2-propenamide (example 5) (1.3mmol) in acetone/water (10:5) was heated to 50° C. After 30 min, sodium hydrosulfite (Na2S2O4) 26.3 mmol) was added slowly. The resulting mixture was heated at reflux (50° C.) for one hour. The mixture was then cooled to room temperature and water was added. The product was isolated by extraction with ethyl acetate. The organic layer washed with 10% aqueous NaHCO3 and then dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. The crude product thereby obtained was recrystallized from 2-propanol to yield the title compound, melting point 92-94° C., in 48% yield.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureThe mixture was then cooled to room temperature
  3. washThe organic layer washed with 10% aqueous NaHCO3
  4. dry with materialdried over anhydrous Na2SO4
  5. customThe solvent was removed under reduced pressure
  6. customThe crude product thereby obtained
  7. customwas recrystallized from 2-propanol