Adamantylpyridine binuclear complex, intermediate and preparation method and application thereof
A technology of adamantyl pyridine and binuclear complexes, applied in the direction of zinc organic compounds, copper organic compounds, drug combinations, etc., can solve the problems of easy hydrolysis by protease, high cost, difficulty in SOD extraction, etc.
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[0046] In the preparation method of the above intermediate, in order to increase the yield of the contact reaction, preferably the contact reaction is carried out below 0°C, and the reaction temperature of the contact reaction is -10-0°C, preferably -3-0°C;
[0047] According to the present invention, in order to make the contact reaction fully proceed, the reaction time of the contact reaction is 3-20 h, preferably 10-15 h.
[0048]The present invention also provides a preparation method for the adamantylpyridine dinuclear complex of the structure shown in formula (I), in the presence of an organic solvent, the intermediate of the structure shown in the formula (L1) and [M(CH 3 COO) 2 ]·H 2 O carries out complex reaction;
[0049]
[0050] In the above formula, M is a divalent metal cation;
[0051] Preferably, M is Cu 2+ or Zn 2+ ;
[0052] More preferably, the [M(CH 3 COO) 2 ]·H 2 O is Cu(CH 3 COO) 2 ·H 2 O.
[0053] According to the present invention, the o...
preparation example 1
[0063] Preparation of 1-adamantanyl chloride:
[0064] In a 250mL round-bottomed flask, add 10.0mmol of 1-adamantanecarboxylic acid solid and 60mL of anhydrous toluene solvent in sequence, and slowly add 20mL of thionyl chloride dropwise after magnetic stirring to dissolve, reflux at 80°C for 8 hours, and cool to 20°C , the solvent was removed by rotary evaporation, and 10 mL of anhydrous toluene was added three times, and the solvent and excess thionyl chloride were removed by rotary evaporation to obtain a light yellow crystalline powder.
Embodiment 1-1
[0066] The preparation of the intermediate of structure shown in formula (L1):
[0067]
[0068] In a 100mL round-bottomed flask, at 0°C, add 5.0mmol of 1-adamantanyl chloride and 25mL of anhydrous toluene in turn. After magnetically stirring to dissolve, add 10mmol of anhydrous potassium carbonate, and slowly add 6.3mmol of 2-aminopyridine dropwise. , reacted under ice-bath conditions for 12 hours, filtered, and obtained 1.154 g of a light yellow crude product after removing the solvent by rotary distillation under reduced pressure. The crude product was recrystallized from a mixed solvent of ethyl acetate and ether to obtain a white powder. Recrystallized in a mixed solvent of ethyl acetate and petroleum ether (v / v=1:3) to obtain 0.873 g of white powder with a yield of 68%. Its detection data are as follows.
[0069] The white powder was subjected to elemental analysis, and the result was C 16 h 20 N 2 O: C, 75.12%; N, 10.87%; H, 7.68%, theoretically calculated value...
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