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With palladium diacetate; caesium carbonate; In N,N-dimethyl-formamide; at 20 - 80℃;
Intermediate 1 (43mg, 0.2mmol), Pd (OAc)2(2.3mg, 0.01mmol) and Cs2CO3(130mg, 0.4mmol) dissolved in 10 ml DMF (dimethylformamide) solution, stirred at room temperature for 5 minutes was heated to 80 deg.] C, while below the liquid continuously fed to the oxygen;Step C, by TLC (thin layer chromatography) to detect the reaction process,Procedure D, after completion of the reaction, 20mL of deionized water was added; the solution was filtered, the precipitate was rinsed with water, then redissolved in 5mL 20mLCH2Cl2The first with 1% EDTA solution rinse (AIM: To remove excess palladium catalyst), then wash with water;Step E, the organic phase was dried over anhydrous Na2SO4After drying, the solvent was distilled off under reduced pressure, to give a yield of 97% of the final compound HBO.
82%
With sodium cyanide; oxygen; In N,N-dimethyl-formamide; at 20℃; for 8h;
General procedure: An imine 3 (0.50 mmol: 1.0 equiv) and NaCN (2.5 mg; 0.050 mmol; 10 mol %) were dissolved in DMF (2.0 mL). The reaction mixture was stirred at room temperature in an open flask and monitored by TLC. On the complete consumption of the imine, the reaction mixture was quenched with H2O, and extracted with Et2O. The organic layer was collected, dried over MgSO4, and concentrated. The crude product was purified by column chromatography
General procedure: Zn(HPB)(Clq) was prepared by adding a solution of zinc sulfate (1mM) in water to a solution of the 5-chloro-8-hydroxyquinoline(1mM) and 2-(2-hydroxyphenyl)benzoxazole (1mM) in acetonitrile. The pH was adjusted to neutral by adding ammonia solution. After stirring the mixture for 2h at 60C on a magnetic stirrer, a crude product precipitated from the solution. The cream colored precipitate was washed with deionised water to remove the excess metal ions and then recrystallized with acetonitrile, to give a pure Zn(HPB)(Clq) as shown in Scheme 1. The recrystallized materials were further purified by vacuum sublimation technique. The chelate gave yellow fluorescence under UV light. Zn(HPB)(Cl2q) was prepared as shown in the reaction, following the above-said procedure using <strong>[773-76-2]5,7-dichloro-8-hydroxyquinoline</strong> instead of 5-chloro-8-hydroxyquinoline. The chelate gave orange-yellow fluorescence under UV light.
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