反应 #3385080
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US06794378B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Triethylamine (35 ml) was added into dimethylformamide (50 ml) including 2-chloro-5-nitropyridine (1) (9.5 g, 60 mmol) and para-phenylenediamine hydrochloride (10.9 g, 60 mmol), and stirred at the room temperature for 14 hours. After the reaction having been completed, the solution was poured into water, and the resultant solid was filtered and then N-(5-nitropyridin-2-yl) para-phenylenediamine was obtained as a brown solid. This solid was dissolved in ethanol (800 ml) and added with 5%-palladium carbon (2 g) so as to cause a hydrogen substitution, and then reduced at 70° C. under the normal pressure for 6 hours. After the reaction having been completed, the celite filtering was applied to remove the palladium carbon, and then it was washed by using a mixed solvent of ethyl acetate and hexane, thus obtained N-(5-amino-pyridin-2-yl) para-phenylenediamine (8.8 g, 75%). the resultant solid was filtered
来源 ID: ord-9f3add445076453383401c22a156d5df