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With copper(l) iodide; tetrakis(triphenylphosphine) palladium(0); triethylamine; In tetrahydrofuran; at 70℃; under 7.50075e-05 Torr; for 10h;Inert atmosphere;
In this embodiment, a white light emitting material is synthesized, and the chemical structure formula of the white light emitting material is as follows:The preparation method includes the following steps:(1) 5.0 mmol of tris (4-iodophenyl) amine, 21.0 mmol of methyl 4-ethynylbenzoate, 30.0 mL of tetrahydrofuran,7.0mL of triethylamine was placed in a 100mL double-necked flask equipped with a stir bar and connected to a reflux tube;(2) Vacuum the reaction mixture with a vacuum pump so that the pressure reaches 1x10-2Pa,Pass in nitrogen, repeat pumping and nitrogen three times to maintain the nitrogen atmosphere of the reaction system;(3) adding 0.125 mmol of tetra (triphenylphosphine) palladium and 0.8 mmol of cuprous iodide to the above reaction solution under a nitrogen environment;(4) The above reaction mixture was heated to 70 C. under the protection of nitrogen and kept at reflux for 10 hours.The solvent was then evaporated to dryness on a rotary evaporator and washed with a small amount of ethyl acetate to give a yellow powder.Purified by column chromatography (silica gel column model: Yantai Jiangyou F-254 200-300 mesh,The mobile phase was a mixed solvent of methylene chloride and n-hexane, and the volume ratio of methylene chloride to n-hexane was 1:30) to obtain a white solid powder, that is, the white light-emitting material.The obtained white solid powder was characterized by hydrogen spectrum and carbon spectrum.
At -78C, n-butyllithium (2.4 mL, 2.5 mol / L, 1.2 equivalents) was added dropwise to a tetrahydrofuran solution (15 mL) of methyl 4-ethynylbenzoate (800.9 mg, 1.0 equivalent) and reacted for 1 h. , then isopropanol pinacol borate (1.2 mL, 1.2 equivalents) was added dropwise to the mixed solution, The reaction was continued for 2h, quenched by the addition of a 1,4-dioxane solution of hydrogen chloride (1.9mL, 4M indioxane, 1.5 equivalents), and the reaction was warmed to room temperature. After the solvent was rotary evaporated, it was prepared into an acetone solution (0.3M), Add potassium peroxymonosulfonate solution (0.5M, 4.6107g, 1.5 equivalents), transfer to 50 C. and stir for 12 h, isolate and purify to obtain 660.2 mg of 2- (4-methoxycarbonyl) phenyl) acetic acid with a purity of 68%.
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