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A kind of heteropolyvanadate compound and preparation method thereof

A heteropolyvanadate compound, crystallization technology, applied in the direction of organic chemistry methods, chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, etc., can solve the problem of high price, uncertain safety of immunotherapy, The problem of drug resistance is difficult and other issues

Active Publication Date: 2021-04-06
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the clinical treatment of tumors mainly adopts surgery, radiotherapy, chemotherapy and other methods, but the side effects of chemotherapy drugs are relatively large; although targeted therapy drugs are sensitive, the problem of drug resistance is very difficult and expensive; the safety of immunotherapy is uncertain

Method used

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  • A kind of heteropolyvanadate compound and preparation method thereof
  • A kind of heteropolyvanadate compound and preparation method thereof
  • A kind of heteropolyvanadate compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Preparation of a heteropolyvanadate compound

[0023] VCl 4 (20 mg, 0.104 mmol) and organic ligand 4,4,4-triazine-2,4,6-tribenzoic acid (abbreviated as: H 3 TATB, 25 mg, 0.057 mmol) was dissolved in 2 mL N,N-dimethylformamide (DMF) and 0.5 mL acetonitrile solution, stirred at room temperature for 30 minutes, and then transferred to a polytetrafluoroethylene reactor for crystallization at 130 °C for 48 hour, after the program was cooled to room temperature, the green crystals were isolated, washed with DMF, and dried at room temperature to obtain the target product (yield 69%, based on H 3 TATB); molecular formula [NH 2 (CH 3 ) 2 ] 12 [(V 5 o 9 Cl) 6 (TATB) 8 ].

Embodiment 2

[0024] Example 2 Structural Analysis and Basic Characterization of Compounds

[0025] Compound [NH 2 (CH 3 ) 2 ] 12 [(V 5 o 9 Cl) 6 (TATB) 8 ] crystallized in the cubic crystal system, the space group is Fm-3m ,Cell parameters a = b = c =40.0473(9)Å, α=β=γ=90°, V=64227(4)Å 3 . The compound is a nanomolecular cage structure with an octahedral configuration, and each vertex of the octahedron is composed of [V 5 o 9 Cl]-built pentanuclear vanadyl clusters, each vanadyl cluster is bridged by four TATB organic ligands through terminal oxygen, and each TATB organic ligand is bridged by three carboxyl groups to three [V 5 o 9 Cl] clusters, each nanomolecular cage consists of six [V 5 o 9 Cl] clusters are bridged by eight organic ligands, TATB, to form a nanomolecular cage with an octahedral configuration. The size of the nanomolecular cage is 3.2 nm. Adjacent nanomolecular cages form a cubic packing pattern in space, forming a three-dimensional supramolecular comp...

Embodiment 3

[0031] Example 3 In vitro experiments to detect the inhibitory effect of compounds on tumor cells

[0032] 1. Experimental materials

[0033] Tumor cells: SMMC-7721 (human liver cancer cells)

[0034] MCF-7 (human breast cancer cells)

[0035] A549 (human lung cancer cells)

[0036] HL-60 (human leukemia cells);

[0037]Culture medium: RPMI640 medium containing 10% calf serum (medium for culturing SMMC-7721 cells), DMEM medium containing 10% calf serum (medium for cultivating MCF-7 and A549 cells), containing 10% IMEM medium (medium for culturing HL-60 cells) with calf serum.

[0038] 2. Experimental method

[0039] Resuscitate the cells by conventional methods, and adjust the cell concentration to 4×10 4 Cells / ml (SMMC-7721 cells, MCF-7 cells), 8×104 cells / ml (A549 cells), 1.5×105 cells / ml (HL-60 cells); 96-well plate culture, add cell suspension to each well 100 μl was cultured at 37°C and 5% CO2 for 24 hours, and then the culture solution of the corresponding cells w...

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Abstract

The invention discloses a heteropolyvanadate compound, the molecular formula is [NH 2 (CH 3 ) 2 ] 12 [(V 5 o 9 Cl) 6 (TATB) 8 ]; The preparation method is: VCl 4 and 4,4,4-triazine-2,4,6-tribenzoic acid were dissolved in 2mL N,N-dimethylformamide and 0.5 mL acetonitrile solution, stirred at room temperature; crystallized at 125~135°C for 40 ~60 hours; cool down, separate green crystals, wash, and dry at room temperature to obtain a heteropolyvanadate compound; the results of in vitro experiments show that the salt is effective on half of SMMC‑7721, MCF‑7, A549, HL‑60 cells The inhibitory concentrations were 0.67 μmol / L, 0.44 μmol / L, 0.48 μmol / L, and 2.09 μmol / L; in vivo experiments showed that the salt could reduce the tumor weight of Hep-A-22 liver cancer-bearing mice.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis of drugs, and in particular relates to a heteropolyvanadate compound and a preparation method thereof. Background technique [0002] In recent years, the incidence of malignant tumors has been increasing year by year, while the age of onset has been decreasing, and the mortality rate is high, seriously endangering human health. According to statistics from the American Cancer Society in September 2018, there were 18.1 million new cancer cases and 9.6 million cancer deaths worldwide. At present, the clinical treatment of tumors mainly adopts surgery, radiotherapy, chemotherapy and other methods, but the side effects of chemotherapy drugs are relatively large; although targeted therapy drugs are sensitive, the problem of drug resistance is very difficult and expensive; the safety of immunotherapy is uncertain. If a cost-effective anti-tumor drug can be developed, it will be a boon for ca...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/00A61P35/00A61P35/02A61K31/555
CPCA61P35/00A61P35/02C07B2200/13C07F9/005
Inventor 李娟郑雁王新龙李金华赵尧李婉玲
Owner JILIN UNIV
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