反应 #3740543
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08742043B2
反应条件: temp:110.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Trisdibenzylideneacetonedipalladium (0.276 g, 0.3 mmol) and tri-tert-butylphosphine (0.121 g, 0.6 mmol) were put into a flask, and then dissolved in 40 mL of toluene. Subsequently, 2-biphenylamine (2.53 g, 15 mmol), 1-bromo-2-methoxybenzene (2.81 g, 15 mmol) and tert-butoxy sodium (2.16 g, 22.5 mmol) were added into the flask, and then refluxed at a temperature of 110° C. for 12 hours. After cooling the flask including the reactant mixture to room temperature, the reactant mixture was washed using an ammonium chloride aqueous solution (150 mL) to separate an organic layer. The separated organic layer was washed with distilled water three times, and was then dried with magnesium sulfate. Thereafter, residues from which volatile components were removed at reduced pressure were purified using a silica gel chromatography tube in a mixed solvent of hexane and ethylacetate (1:10), and were then recrystallized in normal hexane to produce 3.39 g of N-(2′-methoxyphenyl)biphenyl-2-amine. After cooling the flask to room temperature the reactant mixture was washed to separate an organic layer The separated organic layer was washed with distilled water three times was then dried with magnesium sulfate Thereafter, residues from which volatile components were removed at reduced pressure were purified were then recrystallized in normal hexane
来源 ID: ord-e918e3ab32194376914d423e3d58f7aa