反应 #992719

反应方程式

2,7-bis(acetylamino)dibenzodioxin

3-iodopyridine

potassium carbonate

quinoline

→

crude product

2,7-bis(N-3-pyridylacetylamino)dibenzodioxin

溶剂

water

methylene chloride

反应条件

后处理

1. 1
   温度was heated
2. 2
   温度The reaction mixture was cooled to room temperature
3. 3
   其他a precipitate was separated by filtration
4. 4
   workup.ADDITIONTo the filtrate was added 100 ml of water
5. 5
   其他the organic layer was separated from the aqueous layer
6. 6
   浓缩The organic layer was concentrated
7. 7
   其他dried under reduced pressure

实验过程

A slurry prepared from 7.0 g (0.023 mole) of 2,7-bis(acetylamino)dibenzodioxin, 12.0 g (0.059 mole) of 3-iodopyridine, 9.8 g (0.051 mole) of copper (I) iodide, 12.9 g (0.093 mole) of potassium carbonate, and 230 ml of quinoline was heated with stirring at 170° C. for 48 hours. The reaction mixture was cooled to room temperature, 100 ml of methylene chloride and 100 ml of water were added, and a precipitate was separated by filtration. To the filtrate was added 100 ml of water and the organic layer was separated from the aqueous layer. The organic layer was concentrated and dried under reduced pressure to give 23.5 g of a crude product which was used without purification in the next reaction.

来源