Реакция #992718

Уравнение реакции

2,7-bis(acetylamino)dibenzodioxin

iodobenzene

potassium carbonate

quinoline

→

crude product

2,7-bis(N-phenylacetylamino)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 500 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 34.3 g (0.115 mole) of 2,7-bis(acetylamino)dibenzodioxin, 96.4 g (0.576 mole) of iodobenzene, 48.2 g (0.253 mole) of copper (I) iodide, 63.6 g (0.460 mole) of potassium carbonate, and 1500 ml of quinoline was heated with stirring at 170° C. for 48 hours. The reaction mixture was cooled to room temperature, 500 ml of methylene chloride and 500 ml of water were added, and a precipitate was separated by filtration. To the filtrate was added 500 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 79.4 g of a crude product which was used without purification in the next reaction.

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