HRID424353

反应详情

EQUATION

反应方程式

HRID 424353 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 4-methoxy-3-nitrobenzyl sulfonylacetic acid (4.5 g, 15.5 mmol) in 30 mL of glacial acetic acid was added 2,4,6-trimethoxybenzaldehyde (3.05 g, 15.5 mmol) and a catalytic amount of benzylamine (0.6 mL). The resulting mixture was heated at reflux temperature for 6 h. The reaction mixture was then concentrated under reduced pressure to yield a gummy material. The gum was triturated with 2-propanol to yield a solid product. The solid product was recrystallized from a mixture of acetic acid and 2-propanol to provide the 2-((E)-2-(4-methoxy-3-nitrobenzylsulfonyl)vinyl)-1,3,5-trimethoxybenzene product in 28% yield. m.p. 186-187° C.

WORKUP

后处理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux temperature for 6 h
  3. concentrationThe reaction mixture was then concentrated under reduced pressure
  4. customto yield a gummy material
  5. customThe gum was triturated with 2-propanol
  6. customto yield a solid product
  7. customThe solid product was recrystallized from a mixture of acetic acid and 2-propanol