Copper nitrate complex taking 1-(2-pyridine)-9-benzyl-beta-carboline as ligand as well as synthesis method and application of copper nitrate complex
A synthesis method and technology of copper nitrate, applied in the field of medicine, can solve the problems such as synthesis method and application that have not yet been seen
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Embodiment 1
[0044] Embodiment 1: The compound shown in formula (II) is the synthesis of 1-(2-pyridine)-9-benzyl-β-carboline (L)
[0045] 1) Add 1.6g (10mmol) tryptamine, 1.1g (10mmol) pyridine-2-carbaldehyde and 50ml toluene into a 150ml round bottom flask, add a water separator and a condenser tube to form a component water reflux device, heat and reflux for 4 hours, wait After the reaction, the solvent was evaporated to dryness, and the residue was recrystallized with 100ml of n-hexane to obtain compound 1 (2.3g, yield 92%);
[0046] 2) Add 2.5g (10mmol) compound 1, 2.5g palladium carbon (10%Pd / C) and 100ml p-xylene to a 250ml round bottom flask, heat to reflux, and use thin layer chromatography to track and detect until the end of the reaction, and let stand Suction filtration and the filtrate was evaporated to dryness, and the resulting residue was purified by silica gel column chromatography (V 石油醚 :V 二氯甲烷 =1:1), to obtain compound 2 (2.1g, yield 86%);
[0047] 3) Add 0.24g (10mmo...
Embodiment 2
[0055] Embodiment 2: the synthesis of ligand L
[0056] Repeat Example 1, the difference is:
[0057] In step 2), with Mn(Ac) 3 Instead of palladium carbon, glacial acetic acid instead of p-xylene, control Mn(Ac) 3 The amount of compound 1 added was twice that of compound 1, and the reaction was carried out at 70°C. TLC was tracked and detected until the end of the reaction, and then the pH of the system was adjusted to 7 with ammonia water, extracted three times with ethyl acetate, and the organic phases were combined. , evaporate the solvent to dryness, and the resulting residue is applied to a silica gel column (chromatographic purification (V 石油醚 :V 二氯甲烷 =1:1), compound 2 was obtained.
[0058] The product obtained in this example was analyzed by H NMR, C NMR and high resolution mass spectrometry, and it was determined to be the target product 1-(2-pyridine)-9-benzyl-β-carboline.
Embodiment 3
[0059] Embodiment 3: the synthesis of ligand L
[0060] Repeat Example 2, the difference is:
[0061] In step 2), with Pb(Ac) 4 instead of Mn(Ac) 3 , to control Pb(Ac) 4 The amount of added is 5 times the amount of compound 1, and the reaction is carried out at 60°C.
[0062] The product obtained in this example was analyzed by H NMR, C NMR and high resolution mass spectrometry, and it was determined to be the target product 1-(2-pyridine)-9-benzyl-β-carboline.
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