HRID1245843

反应详情

EQUATION

反应方程式

HRID 1245843 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

2-[(Aminocarbonyl)amino]-5-bromo-3-thiophenecarboxamide (11.75 g) was stirred in 1,2-dimethoxyethane (500 ml) and saturated aqueous sodium bicarbonate solution (100 ml), and 4-formylphenyl boronic acid (10 g) was added. The flask was flushed with argon, and tetrakis-(triphenylphosphine)palladium(0) (5.1 g) was then added. The reaction was stirred at 90° C. for 2 h, then cooled and evaporated under reduced pressure. The residue was treated with dichloromethane (200 ml) and 2N sodium hydroxide solution (100 ml), and stirred for twenty minutes. The resulting solid was then isolated by filtration, and purified by trituration with ethanol (100 ml), giving the product as a pale green solid (5.75 g).

WORKUP

后处理

  1. customThe flask was flushed with argon, and tetrakis-(triphenylphosphine)palladium(0) (5.1 g)
  2. additionwas then added
  3. temperaturecooled
  4. customevaporated under reduced pressure
  5. additionThe residue was treated with dichloromethane (200 ml) and 2N sodium hydroxide solution (100 ml)
  6. stirringstirred for twenty minutes
  7. customThe resulting solid was then isolated by filtration
  8. custompurified by trituration with ethanol (100 ml)