반응 #992719

반응 방정식

2,7-bis(acetylamino)dibenzodioxin

3-iodopyridine

potassium carbonate

quinoline

→

crude product

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

용매

water

methylene chloride

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도The reaction mixture was cooled to room temperature
3. 3
   기타a precipitate was separated by filtration
4. 4
   workup.ADDITIONTo the filtrate was added 100 ml of water
5. 5
   기타the organic layer was separated from the aqueous layer
6. 6
   농축The organic layer was concentrated
7. 7
   기타dried under reduced pressure

실험 절차

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.

출처