反応 #640556

反応方程式

4,4′-dibromobenzil

o-phenylenediamine

→

2,3-bis(4-bromophenyl)quinoxaline

収率 92.0%

溶媒

chloroform

反応条件

後処理

1. 1
   洗浄The reaction solution was washed with water
2. 2
   温度after being cooled to room temperature
3. 3
   抽出An aqueous layer was extracted with chloroform
4. 4
   洗浄washed with a saturated saline solution
5. 5
   乾燥The organic layer was dried over magnesium sulfate
6. 6
   ろ過filtered
7. 7
   その他condensed

実験手順

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).

出典