反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe flask was flushed with argon, and tetrakis-(triphenylphosphine)palladium(0) (5.1 g)
- additionwas then added
- temperaturecooled
- customevaporated under reduced pressure
- additionThe residue was treated with dichloromethane (200 ml) and 2N sodium hydroxide solution (100 ml)
- stirringstirred for twenty minutes
- customThe resulting solid was then isolated by filtration
- custompurified by trituration with ethanol (100 ml)