반응 #640556

반응 방정식

4,4′-dibromobenzil

o-phenylenediamine

→

2,3-bis(4-bromophenyl)quinoxaline

수율 92.0%

용매

chloroform

반응 조건

후처리

1. 1
   세척The reaction solution was washed with water
2. 2
   온도after being cooled to room temperature
3. 3
   추출An aqueous layer was extracted with chloroform
4. 4
   세척washed with a saturated saline solution
5. 5
   건조The organic layer was dried over magnesium sulfate
6. 6
   여과filtered
7. 7
   기타condensed

실험 절차

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).

출처