Synthesis method of tetraalkyl tetrazaporphyrin metal coordination compound

A technology of tetraalkylporphyrazine and alkylporphyrazine, which is applied in the field of synthesis of metal complexes, can solve the problems of low yield and poor solubility, and achieve high yield, high-efficiency synthesis method, The effect of easy control of reaction conditions

Inactive Publication Date: 2005-05-18
HEILONGJIANG UNIV
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  • Abstract
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Problems solved by technology

[0003] The purpose of the present invention is aimed at the problems of poor solubility and low yield of porphyrazine metal complexes, to design and research a new synthesis method of tetraalkylporphyrazine metal complexes, by adopting ammonium molybdate as catalyst The technical scheme is to synthesize and prepare tetraalkylporphyrazine metal complexes to achieve the purpose of improving the solubility and yield of tetraazaporphyrazine metal complexes

Method used

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  • Synthesis method of tetraalkyl tetrazaporphyrin metal coordination compound
  • Synthesis method of tetraalkyl tetrazaporphyrin metal coordination compound

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Experimental program
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Effect test

Embodiment 1

[0018] As above-mentioned specific synthetic steps:

[0019] (1) The raw material that takes by weight percentage as follows: Tetraalkyl porphyrazine tetra-tert-butyl porphyrazine 1.5%, 1,2,4-trichlorobenzene 96%, anhydrous cuprous chloride 2%, ammonium molybdate 0.5%, the sum of the total weight percentages is 100%;

[0020] (2) Dissolve tetra-tert-butyl porphyrazine, anhydrous cuprous chloride, and ammonium molybdate in 1,2,4-trichlorobenzene, boil for 4 hours, and monitor the reaction with electronic absorption spectroscopy Proceeding situation, reaction formula is as above.

[0021] (3) After the reaction, the solvent was distilled off under reduced pressure, and a silica gel column was used for chromatographic separation to obtain a deep purple tetra-tert-butylporphyrazine copper complex.

[0022] Yield: 90.8%, melting point>200°C.

[0023] The characteristic absorption peaks of the infrared spectrum are: 2955, 2922, 2863, 1247, 1200, 771, 843, 1010 (the strongest abso...

Embodiment 2

[0031] (1) The raw material that takes by weight percentage as follows: tetraalkyl porphyrazine selects tetra-tert-butyl tetraazaporphyrin 1.5%, 1,2,4-trichlorobenzene 93%, anhydrous lead acetate 5%, Ammonium molybdate 0.5%, the sum of the total weight percentages is 100%;

[0032] (2) tetra-tert-butyl porphyrazine, anhydrous lead acetate, ammonium molybdate were dissolved in 1,2,4-trichlorobenzene, under boiling conditions for 10 hours, monitored the progress of the reaction with electronic absorption spectroscopy, The reaction formula is as above.

[0033] (3) After the reaction, the solvent was distilled off under reduced pressure, and the silica gel column was used for chromatographic separation to obtain a dark green tetra-tert-butylporphyrazine lead complex.

[0034] Yield: 94.3%, melting point > 200°C.

[0035] The characteristic absorption peaks of infrared spectrum are: 2953, 2915, 2863, 1246, 1203, 771, 843, 991 (the strongest absorption), 1070 (double peak), 1358,...

Embodiment 3

[0043] (1) Weigh the following raw materials in percent by weight: tetraalkyl porphyrazine tetra-tert-butyl tetraazaporphyrin 1.5%, 1,2,4-trichlorobenzene 94%, anhydrous nickel chloride 4 %, ammonium molybdate 0.5%, the sum of the total weight percentages is 100%;

[0044] (2) Dissolve tetra-tert-butyl porphyrazine, anhydrous nickel chloride, and ammonium molybdate in 1,2,4-trichlorobenzene, boil for 12 hours, and monitor the progress of the reaction with electronic absorption spectroscopy In this case, the reaction formula is as above.

[0045] (3) After the reaction, the solvent was distilled off under reduced pressure, and the silica gel column was used for chromatographic separation to obtain a dark purple tetra-tert-butylporphyrazine nickel complex.

[0046] Yield: 93.4%, melting point > 200°C.

[0047] The characteristic absorption peaks of infrared spectrum are: 2954, 2922, 2863, 1252, 1203, 772, 843, 1013 (the strongest absorption), 1079 (double peak), 1358, 1387, 14...

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Abstract

The synthesis method of tetraalkylporphyrazine metal complexes relates to a chemical and chemical synthesis processing method, which comprises tetraalkylporphyrazine, anhydrous metal salt, ammonium molybdate and 1,2,4-trichlorobenzene Weigh them according to their respective weight percentages, dissolve the first three raw materials in 1,2,4-trichlorobenzene, react at room temperature to 250°C for 30 minutes to 20 hours, distill off the solvent under reduced pressure, and conduct the reaction on a silica gel column. Chromatographic separation to obtain tetraalkylporphyrazine metal complexes; the method is simple and efficient, the reaction conditions are easy to control, there is no special requirement on the reaction system, and the yield is high, which is suitable for both laboratory preparation and industrialization production, and its complexes have high solubility.

Description

technical field [0001] The present invention relates to a kind of synthetic method of metal complex, especially about tetra-tert-butyl porphyrazine metal complex and its synthetic method, the method of the present invention can be widely used in tetraalkyl porphyrazine metal complex complex synthesis. Background technique [0002] Porphyrazine and its derivatives have a multi-electron π-conjugated system with a planar configuration, and can form complexes with various metal ions. Various substituent groups can be connected to the periphery and axial direction of its macrocycle. The modifiability of the structure makes porphyrin and its derivatives have many excellent physical and chemical properties. At the same time, it has good thermal and chemical stability, making porphyrin compounds widely used in biology, bionics, and materials science. , medicinal chemistry, electrochemistry, photophysical chemistry and other fields have very broad application prospects as anticancer...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D487/22C07F1/08C07F3/00C07F5/06C07F7/00C07F13/00C07F15/00
Inventor 陈志敏吴谊群左霞
Owner HEILONGJIANG UNIV
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