تفاعل #992718

ord-9374108a7280443e8dba6ab2123f1ac4

المذيبات

ظروف التفاعل

درجة الحرارة
170°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةThe reaction mixture was cooled to room temperature
  3. 3
    أخرىa precipitate was separated by filtration
  4. 4
    workup.ADDITIONTo the filtrate was added 500 ml of water
  5. 5
    أخرىthe organic layer was separated from the aqueous layer
  6. 6
    تركيزThe organic layer was concentrated
  7. 7
    أخرىdried under reduced pressure

الإجراء التجريبي

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.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08012606B2uspto-grants-2011_09