反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
In a 200 mL three-neck flask were put 3.0 g (7.8 mmol) of 2-(3-bromophenyl)dibenzo[f,h]quinoxaline, 2.6 g (8.6 mmol) of 3-(dibenzothiophen-4-yl)phenylboronic acid obtained in Step 2, 0.24 g (0.78 mmol) of tri(ortho-tolyl)phosphine (P(o-tolyl)3), 78 mL of toluene, 7.8 mL of ethanol, and 12 mL of 2.0 M potassium carbonate aqueous solution. The mixture was degassed by being stirred under reduced pressure, and the air in the flask was replaced with nitrogen. To the mixture was added 35 mg (0.16 mmol) of palladium(II) acetate. The mixture was stirred at 80° C. under a nitrogen stream for 8 hours. After a predetermined period of time had elapsed, the precipitated solid was separated by filtration to give a yellow solid. The solid was washed with water and ethanol, toluene was added thereto, and the resulting mixture was stirred while being heated. The toluene solution was suction-filtered to give 3.1 g of 2-[3′-(dibenzothiophen-4-yl)biphenyl-3-yl]dibenzo[f,h]quinoxaline (abbreviation: 2mDBTBPDBq-II) as a yellow solid (yellow powder) in a yield of 71%.
WORKUP
后处理
- customIn a 200 mL three-neck flask were put
- customThe mixture was degassed
- stirringThe mixture was stirred at 80° C. under a nitrogen stream for 8 hours
- waitAfter a predetermined period of time had elapsed
- customthe precipitated solid was separated by filtration
- customto give a yellow solid
- washThe solid was washed with water and ethanol, toluene
- additionwas added
- stirringthe resulting mixture was stirred
- temperaturewhile being heated
- filtrationThe toluene solution was suction-filtered