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With [(S)-BINAP]PdBr2; hydrogen; In dichloromethane; at 120℃; under 41372.9 Torr; for 48h;Autoclave;
General procedure: From a Schlenk tube under nitrogen atmosphere, a solution of a-diketone (1mmol), aniline (1mmol), [(S)-BINAP]PdBr2] (0.025 mol), in CH2Cl2 (10 ml) was transferred to a 45 ml stainless steel Parr vessel and the vessel was pressurized with 800 psi of hydrogen gas. The reactor was placed in a preheated oil bath at 120 °C with magnetic stirring over different periods of time (24, 48h). The reaction mixture was purified by column chromatography using hexane and methylene chloride as eluents and was analyzed by GC-MS. The formation of intermediates involved in the process was achieved by varying the reaction time (12, 24h), and these intermediates were purified by column chromatography with hexane and ethylacetate as eluents.
General procedure: All materials were dried for one day at 120 C. Chloride and carbonyl derivatives were introduced into a Schlenk of 30 mL. Products were put in vacuo, then under nitrogen. An appropriate volume of anhydrous DMF was added after 10 min of nitrogen bubbling. The solution was vigorously stirred for 20 min at -20 C. TDAE was added slowly under inert atmosphere. The reaction was stirred for one hour. The second reaction phase was performed at rt or at temperature according to procedure of synthesis. The reaction was hydrolysed with distilled water after TLC analysis clearly showed that the chloride 1 had been totally consumed. The aqueous solution was extracted with dichloromethane and the combined organic layers washed with brine then dried on MgSO4.
With iron oxide; choline chloride; ammonium acetate; urea; at 60℃;Green chemistry;
General procedure: A mixture of benzil (1 mmol), aldehyde (1 mmol) primary amine(1 mmol), ammonium acetate (1 mmol) and eutectic mixture stabilized ferrofluids (0.05 g of Fe3O4 in 1 mL of urea-choline chloride based eutectic mixture) was heated at 60 °C with stirring for 2?6 h.After completion of the reaction, the mixture was cooled to room temperature and water was added and products recrystallized in ethanol. All compounds were characterized on the basis of their spectroscopic data (IR, NMR) and by comparison with those reported in the literature
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