Réaction #992718
ord-9374108a7280443e8dba6ab2123f1ac4
Équation de réaction
2,7-bis(acetylamino)dibenzodioxin
iodobenzene
potassium carbonate
quinoline
→
crude product
2,7-bis(N-phenylacetylamino)dibenzodioxin
Réactifs
Solvants
Conditions de réaction
Température
170°CELSIUS
Conditions détaillées
See reaction.notes.procedure_details.
Traitement
- 1Températurewas heated
- 2TempératureThe reaction mixture was cooled to room temperature
- 3Autrea precipitate was separated by filtration
- 4workup.ADDITIONTo the filtrate was added 500 ml of water
- 5Autrethe organic layer was separated from the aqueous layer
- 6ConcentrationThe organic layer was concentrated
- 7Autredried under reduced pressure
Mode opératoire
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.