반응 #1516510

반응 방정식

9-phenanthreneboronic acid

2,7-dibromonaphthalene

dimethoxyethane

sodium carbonate

→

7-bromo-2-(9-phenanthrenyl)naphthalene

수율 38.7%

용매

water

toluene

반응 조건

후처리

1. 1
   추출extracted with toluene
2. 2
   세척After washing with water
3. 3
   건조the organic phase was dried over magnesium sulfate
4. 4
   기타Then, the toluene was removed by distillation under reduced pressure
5. 5
   기타the residue was purified by silica gel chromatography

실험 절차

In argon atmosphere, a mixture of 18.64 g (83.9 mmol) of 9-phenanthreneboronic acid, 30.00 g (104.9 mmol) of 2,7-dibromonaphthalene, 4.85 g (4.2 mmol) of tetrakis(triphenylphosphine)palladium (0), 200 ml of dimethoxyethane, 200 ml of toluene, and 106 ml of a 2 M sodium carbonate was stirred at a bath temperature of 85° C. for 7 h. The reaction mixture was added with water and extracted with toluene. After washing with water, the organic phase was dried over magnesium sulfate. Then, the toluene was removed by distillation under reduced pressure, and the residue was purified by silica gel chromatography to obtain 12.46 g (yield: 31.0%) of 7-bromo-2-(9-phenanthrenyl)naphthalene.

출처