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Eu(iButCHex)3*4,7-diphenylphenanthroline[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
With sodium hydroxide; In ethanol; water;
General procedure: In the preparation of the Ln(CA)3·Phn and Ln(CA)3·Bpy adducts the 3-N NaOH water solution and an ethanol solution of Phn or Bpy were added to an ethanol solution of CA. Then, a water?ethanol (1:1) solution of LnCl3·6H2O was drop by drop added to the previous mixture at heating in a water bath (at 60?70°C) or sometimes without heating. A molar ratio of the reagents CA: Phn (Bpy): lanthanide chloride: NaOH was equal to 3:1:1:3. The compound Eu(AcCHex)3·Phen was also synthesized by other method involving the preparation of an ethanol solution of a mixture of CA, Phen and EuCl3·6H2O in a molar ratio of 3:1:1 and adjusting the pH value of reaction mixture to 6 with a liquid ammonia. It should be pointed out that the heating of the reaction mixture results in a decrease in the keto/enol ratio of cycloalkanone [37] that promotes a binding of CA with the Ln3+ ion. At the same time, the probability of decomposition of cycloalkanonate anion increases.
With tetrakis(triphenylphosphine) palladium(0); sodium carbonate; In ethanol; water; toluene; for 36h;Reflux; Inert atmosphere;
General procedure: First, the product E2-2 is obtained from E2-1 through the Suzuki cross coupling reaction according to the above route, and then the product E2-2 is sequentially processed according to the above reaction scheme to obtain the product E2-4. E2-4 (6.46g, 17.60mmol), E1-1 (2.64g, 8.00mmol) were added to a 500mL round-bottomed flask, and a mixed system of toluene (150ml), ethanol (50mL) and deionized water (100mL) was used as Solvent, add Na2CO3 (6.12g, 57.78mmol) and Pd(PPh3)4 (1.08g, 0.933mmol) as catalyst, heat under reflux for 36 hours, filter after cooling, and successively use ethanol, dichloromethane/methanol mixed solution for many times The filter cake was washed and further processed by conventional methods to give the final product E-2 (3.22 g, 54% yield).