Реакция #640556

ord-fa8f6dad7ad047a4b8e62d003cb4b1e2

Уравнение реакции

O=C(C(=O)c1ccc(Br)cc1)c1ccc(Br)cc1
4,4′-dibromobenzil
Nc1ccccc1N
o-phenylenediamine
Brc1ccc(-c2nc3ccccc3nc2-c2ccc(Br)cc2)cc1
2,3-bis(4-bromophenyl)quinoxaline
Выход 92.0%

Реагенты

Нет

Растворители

Условия реакции

Температура
80°CELSIUS
Подробные условия
See reaction.notes.procedure_details.

Обработка

  1. 1
    ПромывкаThe reaction solution was washed with water
  2. 2
    Температураafter being cooled to room temperature
  3. 3
    ЭкстракцияAn aqueous layer was extracted with chloroform
  4. 4
    Промывкаwashed with a saturated saline solution
  5. 5
    СушкаThe organic layer was dried over magnesium sulfate
  6. 6
    Фильтрацияfiltered
  7. 7
    Другоеcondensed

Методика

A chloroform solution (200 mL) of 30.0 g (81.5 mmol) of 4,4′-dibromobenzil and 9.00 g (83.2 mmol) of o-phenylenediamine was heated and refluxed at 80° C. for 3 hours under nitrogen atmosphere. The reaction solution was washed with water after being cooled to room temperature. An aqueous layer was extracted with chloroform. This extracted aqueous layer and an organic layer were put together and washed with a saturated saline solution. The organic layer was dried over magnesium sulfate and filtered. The filtrate was condensed to obtain 33 g (yield: 92%) of objective 2,3-bis(4-bromophenyl)quinoxaline as a white solid. Synthetic scheme of Step 1 is shown in the following (d-1).

Источник

DOI: 10.6084/m9.figshare.5104873.v1Патент: US08048540B2uspto-grants-2011_11