Reference of 116632-14-5, These common heterocyclic compound, 116632-14-5, name is 3-Iodonaphthalen-2-amine, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
(1) 1.0748 g (4 mmol) of 2-amino-3-iodophthalene (a) was dissolved in a nitrogen atmosphere.140.0 mg (0.2 mmol)Bistriphenylphosphine palladium dichloride [(Ph3P)2PdCl2], 75.9 mg (0.4 mmol) 40 ml of cuprous iodide (CuI)Slowly add 784.5mg (8mmol) to triethylamine (Et3N) solutionTrimethylsilylacetylene.Stir the reaction at room temperature,After TLC monitors the starting material a completely,Stop stirring,The reaction was quenched by adding 50 ml of saturated ammonium chloride to the reaction system.Extraction of organic phase with dichloromethane(3x100ml),The combined organic layers were washed with 50 ml of water, 50 ml of brine and dried over anhydrous magnesium sulfate.The crude product is passed through silica gelSpectroscopic purification (ethyl acetate: petroleum ether = 1:20),Light yellow solid b (783.6 mg, yield 82%)
The synthetic route of 116632-14-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Tsinghua University; Zhao Liang; Wu Han; (14 pag.)CN108997384; (2018); A;,
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