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With tri-tert-butyl phosphine; palladium diacetate; In para-xylene; for 16h;Reflux;
22 g (79.8 mmol) Of 2,12- dimethyl-10-phenyl -10,12- dihydro-10-aza-indeno - [2,1-b] fluorene,34 g (87 mmol)Of the triazine, and 15.9 ml (15.9 mmol)1 mol / l tree -tert- butylphosphine,tri1.79 g (7.9 mmol)The palladium acetateProtective-p- xylene was suspended in 120 ml of gas under.The reaction mixture was heated for 16 hours under reflux. After cooling, the organic phase was separated off, washed three times with 200 ml of water and evaporated to dryness.The residue was extracted with toluene of high temperature, which was recrystallized from toluene, and finally sublimation at high vacuum.The purity is 99.9%.Yield: 38 g (64 mmol), 80% of the theoretical value.Similarly, the following compounds were obtained
With tetrakis(triphenylphosphine) palladium(0); potassium carbonate; In tetrahydrofuran; water; at 80℃; for 20h;Inert atmosphere;
20 g (56.5 mmol) of Compound 1-1 was dissolved in 0.2 L of THF under a nitrogen condition, and, and 15.1 g (56.5 mmol) of 2-chloro-4,6-diphenylpyrimidine and 0.65 g (0.57 mmol) of tetrakis(triphenylphosphine)palladium were added thereto. The mixed solution was then stirred. 19.5 g (141 mmol) of potassium carbonate saturated in water was added thereto, and refluxed by a heating process performed thereon at a temperature of 80 C. for 20 hours. After the reaction was completed, water was added to the reaction solution, and an extraction process was performed thereon by using DCM. Moisture in the extraction was dried by using anhydrous MgSO4, and the resulting mixture was then filtered and concentrated under reduced pressure. The residue obtained therefrom was separated and purified by flash column chromatography to obtain Compound A-3.
With (1,1'-bis(diphenylphosphino)ferrocene)palladium(II) dichloride; potassium acetate; In tetrahydrofuran; water; at 2080.0℃; for 20.0h;Inert atmosphere;
General procedure: <strong>[1092485-88-5]3,5-dichloro-4-fluorophenyl boronic ester</strong> (1.00 equivalents; CAS 1092485-88-5), 2-chloro-4,6-diphenyl-1,3,5-triazine (1.1 equivalents), Pd(dppf)2Cl2 (0.05 equivalent), and potassium acetate (3.00 equivalents) are stirred under nitrogen atmosphere in a THF/water mixture (ratio of 10:1) at 80 C. for 20 h. The cooled mixture is poured into brine, the precipitated product is filtered off and washed with water and cold ethanol. The product E1-1 is obtained as a solid.
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