Реакция #992719

Уравнение реакции

2,7-bis(acetylamino)dibenzodioxin

3-iodopyridine

potassium carbonate

quinoline

→

crude product

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

Растворители

water

methylene chloride

Условия реакции

Обработка

1. 1
   Температураwas heated
2. 2
   ТемператураThe reaction mixture was cooled to room temperature
3. 3
   Другоеa precipitate was separated by filtration
4. 4
   workup.ADDITIONTo the filtrate was added 100 ml of water
5. 5
   Другоеthe organic layer was separated from the aqueous layer
6. 6
   КонцентрированиеThe organic layer was concentrated
7. 7
   Другоеdried under reduced pressure

Методика

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.

Источник