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With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene; for 7h;Inert atmosphere; Reflux;
Under an argon atmosphere, 1.34 g of Compound F, 2.96 g of <strong>[26608-06-0]3-bromo-dibenzofuran</strong>, 0.27 g of bis(dibenzylideneacetone)palladium(0), 0.088 g of tri-tert-butylphosphine and 3.98 g of sodium tert-butoxide were added to a 500 ml three necked flask, followed by heating and refluxing in 200 ml of a toluene solvent for about 7 hours. After air cooling, water was added to the reactant, an organic layer was separated, and solvents were distilled. The crude product thus obtained was separated using silica gel column chromatography (toluene and hexane) to produce 2.20 g of Compound G as a white solid (Yield 70%). The molecular weight of Compound G thus obtained was measured using FAB-MS, and a value of 577 (C42H27NO2) was obtained. In addition, 1H NMR (CDCl3, 300 MHz) of Compound G was measured, and the chemical shift values expected from the structure of Compound G were obtained. Thus, the synthesis of Compound G was secured. In addition, the glass transition temperature of Compound G was measured using a differential scanning calorimetry, DSC 7020 of Hitachi Hightech Co., and a value of Tg: 100 C. was obtained.
With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene;Reflux;
Put 2.0g of <strong>[1256544-32-7]3-bromonaphtho[2,3-b]benzofuran</strong> (<strong>[1256544-32-7]3-bromonaphtho[2,3-b]benzofuran</strong>),0.9g of [1,1':4',1”-terphenyl]-4-amine ([1,1':4',1”-terphenyl]-4-amine), 1.0g of t-BuONa, After 0.3 g of Pd2(dba)3 and 0.2 ml of (t-Bu)3P were dissolved in 70 ml of toluene, reflux and stirring were performed. The reaction was confirmed by Thin Layer Chromatography (TLC), and the reaction was terminated after adding water. The organic layer was extracted with methylene chloride (MC, Methylene chloride) and recrystallized after filtration under reduced pressure, thereby obtaining 3.1 g of compound 42 (yield 68%).
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