反应 #640556

ord-fa8f6dad7ad047a4b8e62d003cb4b1e2

反应方程式

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
收率 92.0%

反应条件

温度
80°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤The reaction solution was washed with water
  2. 2
    温度after being cooled to room temperature
  3. 3
    萃取An aqueous layer was extracted with chloroform
  4. 4
    洗涤washed with a saturated saline solution
  5. 5
    干燥The organic layer was dried over magnesium sulfate
  6. 6
    过滤filtered
  7. 7
    其他condensed

实验过程

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).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US08048540B2uspto-grants-2011_11