24 results about "Single Crystal Diffraction" patented technology

Cell parameters of the crystal compound are as follows: diffraction data are collected in an omega-theta scanning mode by using MoK alpha rays monochromatized by a graphite monochromator on an Oxford X-ray single crystal diffractometer at the temperature of 273 k, and the crystal compound is characterized in that the crystal belongs to a triclinic system, P-1; the cell parameters are as follows: alpha is equal to 79.857 (3) degrees; beta is equal to 87.082 (3) degrees; gamma is equal to 87.829 (3) degrees; the synthesis method of the crystal chlorine compound (I) comprises the following steps: weighing 0.02 35 g of benzophenone hydrazone and 0.6720 g of 1.0 g of 7-chloroisatin and acetic acid ketone monohydrate complex, putting into a 150mL flask, adding 100.0 mL of chlorobenzene as a solvent, stirring at room temperature for 48 hours, carrying out column chromatography separation, eluting with petroleum ether / dichloromethane (1 / 1), and carrying out vacuum drying to obtain the crystal chlorine compound (I). And naturally volatilizing the collected front component points to obtain the target crystal compound I, namely the 6-bromo-3-diphenylmethylene indoline-2-ketone crystal. The application of the crystal chlorine compound (I) is that the crystal chlorine compound (I) has a relatively strong inhibition effect on epidermophyton flocculent, and the IC50 value of the crystal chlorine compound (I) is 0.063 + / -0.008.

This invention provides a crystallization plate suitable for in-situ X-ray diffraction of biomolecules, comprising: a body and multiple crystallization units formed within the body; each crystallization unit includes a through-hole and a frustum-shaped sample slot support within the through-hole; the lower bottom surface of the frustum-shaped sample slot support is connected to the lower bottom surface of the through-hole, and the upper bottom surface of the frustum-shaped sample slot support is located between the upper top surface and the lower bottom surface of the through-hole; the side surface of the frustum-shaped sample slot support and the side surface of the through-hole form a crystallization buffer bath. The crystallization plate of this invention is applicable to in-situ testing of biomolecular crystals, and features simple operation, good compatibility, high efficiency, and low cost. It can greatly facilitate the rapid collection of single-crystal diffraction data or drug screening at synchrotron radiation crystallography beamlines under room temperature in-situ conditions.

The application relates to the technical field of plant chemistry and active ingredient heterocyclic compounds of traditional Chinese medicine, and discloses a C17 sesquiterpene alkaloid, a preparation method and application, wherein the C17 sesquiterpene alkaloid and a pharmaceutically acceptable salt thereof are shown as formula I; the C17 sesquiterpene alkaloid of formula I is separated from an ethanol extract n-butanol extraction phase of Dendrobium huoshanense stems through three-step operations of silica gel column chromatography, acid solution and base precipitation and recrystallization; the structure of the compound is determined through nuclear magnetic resonance, high-resolution mass spectrometry and single crystal diffraction analysis; experiments show that the C17 sesquiterpene alkaloid can effectively inhibit the survival and proliferation of A549 lung cancer cells, has good anti-lung cancer activity, and can be used for preparing anti-lung cancer drugs.

The invention discloses a pentacyclic triterpene acylhydrazone compound as well as a preparation method and application thereof. A series of oleanolic acid derivatives are synthesized by carrying out structural modification on carboxyl at C28 site of oleanolic acid, structural confirmation is carried out by using 1H NMR, 13C NMR, HRMS and X-ray single crystal diffraction, and the inhibition effect of the pentacyclic triterpenoid acylhydrazone compound on the activity of tumor cells A549, AGS and K562 is evaluated by taking cis-platinum as positive control and adopting a CCK-8 method. Results show that the inhibition effect of the derivatives 5, 6, 9, 10, 16, 21, 27 and 28 on tumor cells is superior to that of cis-platinum. Reference is provided for research of oleanolic acid derivatives and discovery of anti-tumor seedling compounds.

The application relates to the structural composition of a [2+2] photocycloaddition polymer and a preparation method thereof, and relates to the technical field of functional materials. The polymer introduces a closed dodecaborane anion, two polymers are prepared by the application, and the two polymers can both undergo [2+2] cycloaddition under the irradiation of ultraviolet light. The [2+2] cycloaddition of the polymer is verified by nuclear magnetic resonance hydrogen spectrum, single crystal X-ray diffraction spectrum, powder single crystal X-diffraction spectrum, infrared spectrum and the like. The application shows the great potential of a supramolecular organic framework material based on B 12 H 12 2‑ in the field of topological chemistry, and lays a solid foundation for the in-depth research in the field in the future.

The invention discloses a chain-shaped silver complex as well as a preparation method and application thereof. The invention relates to a synthesis method of a chain-like silver complex, which comprises the following steps: carrying out condensation reaction on pyridoxal and p-methylbenzenesulfonyl hydrazide to generate a pyridoxal condensed p-methylbenzenesulfonyl hydrazide ligand, reacting the ligand with silver nitrate, slowly volatilizing the reaction liquid for 3-5 days, and separating out a yellow crystal of the chain-like silver complex. The crystal is subjected to structural analysis by adopting an X-ray single crystal diffraction technology, and the result shows that the crystal is a novel chain-shaped coordination polymer. The chain-shaped silver complex shows remarkable antibacterial activity on staphylococcus aureus, pseudomonas aeruginosa, methicillin-resistant staphylococcus aureus and multi-drug-resistant pseudomonas aeruginosa, and the in-vitro antibacterial effect of the chain-shaped silver complex is superior to that of silver nitrate, a ligand and a methicillin monomer; the application potential of the compound serving as an efficient antibacterial agent in the aspect of replacing or supplementing existing anti-infection drugs is shown. The structure of a pharmaceutically acceptable compound of the chain-shaped silver complex is shown as a formula (I) in the specification.

The utility model relates to a sample holder for a micro-area variable-angle grazing incidence wide-angle scattering test. According to the scheme, a table top used for placing a test material, a Z-axis height reference position and a height adjusting driver used for driving the sample frame to move back and forth along a Z axis are arranged on the sample frame; the radian adjusting driver is used for driving the sample holder to do curve swinging motion along the light path direction and in the direction perpendicular to the light path; the connecting part is matched with a sample table of the single crystal diffractometer; wherein the radian adjusting driver is used for driving the table board to swing, so that the incident angle is controlled. The defects of an existing wide-angle scattering test technology based on single crystal XRD in the aspect of incident angle and height control can be overcome.

The application discloses a kind of isoprenylated phenolic acid Drupanin, single crystal and its separation and purification method and application.The application adopts the combined purification process of dynamic axial column chromatography and preparative chromatography, realizes the efficient enrichment and accurate separation of Drupanin component in propolis;And for the first time, the complete three-dimensional spatial structure of Drupanin is determined by X-ray single crystal diffraction technology;Through in-vitro and in-vivo animal experiments, it is proved that the Drupanin prepared by the application can significantly improve neuroinflammation, oxidative stress and lipid metabolism disorder, and can effectively repair cognitive dysfunction, relieve depression and anxiety symptoms, has the advantages of multi-target, low side effect and significant efficacy, can be widely used in improving cognitive impairment, preventing or treating depression, anxiety and other nervous system diseases Functional products and innovative drug research and development, and has good clinical application value.

The invention discloses a piperine-based pseudo-natural dimer amide alkaloid compound 1 and a piperine-based pseudo-natural dimer amide alkaloid compound 2 as well as a preparation method and medical application thereof. Dimerization of piperine is realized through a visible light catalytic reaction system Ir (ppy) 3 / 465nm LED, and optically pure enantiomers 1a / 1b and 2a / 2b are obtained through acetonitrile-water system preparative HPLC separation and purification in combination with a chiral chromatographic resolution technology. HRESIMS, multi-dimensional NMR and X-single crystal diffraction confirm that the structure of the compound has a unique cyclohexene skeleton and a bis-piperidyl structure. A biological activity research shows that the target compound has a remarkable inhibition effect on LPS-induced RAW264.7 macrophage NO release, the compound 1 shows an excellent curative effect in an imiquimod-induced psoriasis mouse model, and the effect of the compound 1 is superior to that of a positive drug benvitimod. The invention provides a green and efficient photocatalytic synthesis method, and the obtained compound provides candidate molecules for developing multi-target anti-psoriasis drugs.

The present invention discloses Monovir Form VII and a preparation method thereof, and belongs to the field of compound crystal forms. The X-ray powder diffraction spectrum of Monovir Form VII measured using Cu-Kα rays is shown in Figure 1. The Monovir Form VII is prepared by adding isobutanol to Monovir, dissolving it, and then using a cooling crystallization method or a solvent evaporation method to obtain Monovir Form VII crystals. The preparation process is simple, and the obtained crystal form has high purity. It is determined to be a new crystal form, Form VII, through the characterization of XRPD, X-ray single crystal diffraction, DSC, and TG.

The present invention discloses a polycyclic polyisopentenyl phloroglucinol compound and its preparation method and application, belonging to the field of biomedicine technology. The dried aerial part of Hypericum perforatum is used as raw material, and an extract is obtained after diafiltration extraction and concentration, and the extract is suspended in water to obtain a suspension, and a petroleum ether extract is obtained after extraction and concentration; the extract is taken and subjected to positive and reverse phase silica gel column, MCI medium pressure column chromatography, Sephadex LH-20 gel column chromatography separation and high performance liquid chromatography purification to obtain a polycyclic polyisopentenyl phloroglucinol compound, and the structure and configuration of the compound are determined by means of spectral analysis technology, quantum chemical calculation and X-ray single crystal diffraction. This type of compound can inhibit TNF-α protein from exerting an immunosuppressive effect and has the use as an immunosuppressive drug.

This invention provides an X-ray single-crystal diffraction sample sealing device and its usage method. The X-ray single-crystal diffraction sample sealing device includes a base, a sampling tube, and a sealing valve. The base has a chamber extending through its bottom. The sampling tube is airtightly connected to the top wall of the chamber, and its bottom end communicates with the top end of the chamber. The sealing valve is threaded into the chamber and has an internal channel connecting the top and bottom ends of the chamber. A sealing element is provided between the top surface of the sealing valve and the top wall of the chamber, and the sealing element cooperates with the sealing valve to seal the bottom end of the sampling tube. Compared with the prior art, this invention can achieve sealed transfer of air-sensitive samples and has the advantages of simple operation and reusability.

The application discloses a vortioxetine impurity, a preparation method and application thereof, and adopts vortioxetine or a pharmaceutically acceptable salt form thereof as raw material, the raw material is easy to obtain and simple to operate, and the reaction condition is mild. The synthesized impurity is characterized by nuclear magnetic resonance, high-resolution mass spectrometry and X-ray single crystal diffraction, and liver toxicity research shows that the compound disclosed by the application has important significance for researching adverse reactions of vortioxetine. The control sample obtained by the method provided by the application can be used for qualitative and quantitative analysis of the vortioxetine impurity, so that the drug safety of vortioxetine is improved.

The application provides a method for synthesizing an R-10-hydroxy-10-(1H-indol-3-)-9-phenanthrenone compound, which comprises the following steps: mixing a 9,10-phenanthrenequinone compound shown in formula 2, an indole compound shown in formula 3 and a chiral catalyst in an organic solvent, and performing reaction to obtain an R-10-hydroxy-10-(1H-indol-3-)-9-phenanthrenone compound shown in formula 4. The application can obtain the R-10-hydroxy-10-(1H-indol-3-)-9-phenanthrenone compound as a main product, the enantiomeric excess value of which is up to 97%, the yield is good (75%-95%), and the absolute configuration of the target compound is determined as R through X-single crystal diffraction experiment. It is found through cell experiment that a series of synthesized compounds have good antitumor activity, and the application provides a basis for the research of chiral drugs.

The invention relates to a synthetic method of an azabicyclo [3.2. 1] octyl-2-ene derivative, and belongs to the technical field of organic synthesis. The synthetic method of the azabicyclo [3.2. 1] octyl-2-ene derivative comprises the following steps: S1, in an inert atmosphere and at a low temperature, carrying out an addition reaction on N-Boc-nortropinone as a raw material and an aryl lithium reagent to obtain an intermediate IM1; s2, removing a Boc protecting group under an acidic condition to obtain an intermediate IM2; and S3, salifying the intermediate IM2 and chiral mandelic acid, performing fractional crystallization and alkali dissociation to obtain a target enantiomer with high optical purity, culturing an S-mandelate single crystal of a compound (1S, 5R)-(+)-3-(4-chlorphenyl)-8-azabicyclo [3.2. 1] oct-2-ene, and determining the absolute configuration of the compound through single crystal diffraction. The synthesis method disclosed by the invention has the characteristics of simple reaction operation in each step, mild conditions, high yield, good repeatability and suitability for industrial large-scale production.

The present invention belongs to the technical field of fluorescent crystal materials, and discloses a manganese-based pyridine fluorescent crystal material, a preparation method and an application. At room temperature, MnCl2·4H2O, 2-dimethylaminopyridine, and 4-dimethylaminopyridine are used as raw materials, and water, methanol, acetonitrile, etc. are used as solvents; the solvent evaporation method is adopted to synthesize 4 examples of manganese-based pyridine organic-inorganic hybrid compounds; the properties of compounds 1-4 are systematically detected by methods such as infrared testing, X-single crystal diffraction, thermogravimetric analysis, dielectric testing, and fluorescence testing. Compounds 1-3 all belong to the monoclinic system, and the space group is C2 / c. Compounds 2-4 all belong to the triclinic system, and the space group is P-1. Compounds 1-4 all start to decompose at about 376K, proving to have good thermal stability. In the temperature-rising dielectric test, compounds 1-4 start to show dielectric anomalies at 220K, 220K, 220K, and 237K respectively.

The application discloses application of a pyrazole ring trinuclear silver (I) complex in organic molecular structure determination, in particular, application of a 3,5-bistrifluoromethyl pyrazole ring trinuclear silver (I) complex in organic molecular structure determination, and specifically comprises the following steps: synthesizing the pyrazole ring trinuclear silver (I) complex; mixing the pyrazole ring trinuclear silver (I) complex with a sample to be measured, obtaining a co-crystal of the pyrazole ring trinuclear silver (I) complex and the organic molecule to be measured and performing single crystal diffraction analysis, collecting crystal data of the co-crystal; analyzing the crystal structure according to diffraction data of the co-crystal, so as to obtain a chemical structure and a stereo configuration of the organic molecule to be measured. The application can be used for molecular structure determination of a series of non-crystalline compounds and mixture samples.

The present invention relates to an integrated data collaborative acquisition method, device and readable storage medium for small-angle scattering and wide-angle scattering based on a single-crystal diffractometer. The method realizes vertical fixation of the sample and high-precision control of the incident angle by designing two improved sample holders (the first sample holder is for the grazing incidence mode, and the second sample holder is for the transmission mode) to replace the magnetic head structure of the original single-crystal diffractometer. The first sample holder adopts a structure of "fixed plate + vertical backrest + groove" to fix the sample through a rigid connecting piece; the second sample holder adopts a back plate with a detection hole to support the fixation of the substrate-free film. The present invention breaks through the limitation of the traditional test range, eliminates the signal splicing error, realizes the full-dimensional characterization of the material structure, and is applicable to the depth gradient analysis of thin films, free films and bulk samples.

The present application relates to the field of catalysis technology, and particularly relates to a Co(II) based photoelectrode crystalline material, a preparation method and application thereof.The present application provides a Co(II) based photoelectrode crystalline material, a preparation method and application thereof, and a new type of cobalt-based metal hydrogen bond organic framework material is successfully prepared by using H3(5-COTDA) as an organic connecting unit through a solvothermal method.The crystal structure and phase purity of the compound are systematically analyzed and confirmed through X-ray single crystal diffraction, Fourier transform infrared spectroscopy and powder X-ray diffraction and other characterization methods.The photoelectric performance test results show that the Co(II) based photoelectrode crystalline material presents a typical n-type semiconductor behavior and exhibits good photoelectric catalytic activity.

The luteolin is low in bioavailability, and the luteolin is the same as metformin and has a wide effect but a weak effect, so that the clinical application of the luteolin and the metformin (except for reducing blood sugar) is limited. In order to improve the problem, the luteolin and metformin eutectic crystal is prepared in the invention. X-single crystal diffraction and FT-IR (Fourier transform infrared spectroscopy) show that luteolin and metformin are coupled into three-dimensional supramolecular lamellar crystals according to a molar ratio of 1: 1 through hydrogen bonds, DSC (differential scanning calorimetry) shows that the melting point of the three-dimensional supramolecular lamellar crystals is remarkably reduced, and DVS (differential scanning spectroscopy) shows that the three-dimensional supramolecular lamellar crystals have good wettability; compared with luteolin, the dissolution rate of the eutectic crystal is increased by more than 7 times, and the biological bioavailability is increased by more than 10 times; anticancer activity shows that luteolin and metformin have an obvious synergistic effect, and a ester reduction experiment shows that the eutectic crystal obviously improves oleic acid induced HepG2 cell lipid droplet accumulation. According to the invention, triple improvement of solubility, bioavailability and pharmacological activity is realized through co-crystallization, and an innovative solution is provided for clinical application of luteolin and development of metformin non-hypoglycemic indications.

The application belongs to the technical field of organic chemistry, and particularly relates to a preparation method of photocatalytic polysubstituted indole compounds. 1 H NMR, 13 C NMR, HRMS, single crystal X-ray diffraction and other methods are used for characterization and confirmation. The method of the application is that, in the presence of a proton acid, 2-indole methanol is de- aromatized to form an imine cation intermediate, then the intermediate is reacted with alkyl radicals generated by hydrogen atom transfer (HAT) of alkane under the catalysis of tetrabutylammonium decatungstate (TBADT) to obtain 2,3-dialkyl substituted indole compounds I through isomerization. The method has the advantages of simple reaction, high efficiency, few side reactions, high product purity, easy separation and purification, mild conditions, wide application range of substrates, simple raw materials, low cost, applicability to large-scale preparation and good application prospect.

The invention discloses diterpenoid compounds in honeycomb and a preparation method and application thereof.The preparation method comprises the steps that the honeycomb is dried in the air and then ground into powder, extraction is conducted through an organic reagent, purification is further conducted through macroporous resin, sephadex, normal-phase silica gel, reverse-phase silica gel and other column chromatography methods, and the diterpenoid compounds are obtained. A monomeric compound is prepared through semi-preparative high performance liquid chromatography, and finally three diterpenoid compounds with novel structures are obtained through structural identification such as one-dimensional nuclear magnetism, two-dimensional nuclear magnetism, ECD and X-single crystal diffraction. The three diterpenoid compounds provided by the invention can inhibit the generation of nitric oxide in a cell inflammation model, and the IC50 of the compound 1 is superior to that of a positive drug indometacin. In addition, the compound 1 can down-regulate gene expression of inflammatory factors IL-1beta and IL-6, has an inhibition effect stronger than that of indomethacin with the same concentration, has remarkable anti-inflammatory activity, and can be applied to development of drugs for treating gouty arthritis.

The application provides an X-ray single crystal diffraction sample selection device and a use method. The X-ray single crystal diffraction sample selection device comprises a moving frame, a selection table, a microscope, a sample table and a double-layer jet pipe. The selection table is movably arranged on the moving frame. The microscope is arranged on the selection table. The sample table is arranged on an objective table of the microscope. The double-layer jet pipe is arranged on the selection table and is connected with a low-temperature inert gas source and a room-temperature inert gas source respectively. The double-layer jet pipe can jet double-layer inert gas towards the sample table. The inner layer and the outer layer of the double-layer inert gas are the low-temperature inert gas and the room-temperature inert gas respectively. Compared with the prior art, the application can realize selection and rapid transfer of air-sensitive samples and prevent the air-sensitive samples from deteriorating during the selection and transfer.

The invention discloses a portable liquid nitrogen replenishment device of a single crystal diffractometer, and relates to the technical field of liquid nitrogen replenishment device.The portable liquid nitrogen replenishment device comprises a bottom plate and a liquid nitrogen container, a fixing frame is fixedly connected to the upper end of the bottom plate, a moving assembly is arranged on the outer side of the fixing frame, a fixing plate is fixedly connected to the outer side of the fixing frame, and a fixing assembly is arranged in the fixing plate; according to the portable liquid nitrogen supply device of the single crystal diffractometer, the whole device can be lifted and carried through the arranged straps, the telescopic rod is pulled out through the pull rod, and under the action of the universal wheels, the portable liquid nitrogen supply device is convenient to move and carry; due to the fact that the fixing pipe is connected with the two sets of connecting ports respectively, liquid nitrogen supply for the diffractometer is conducted in sequence without interruption, the problem caused by insufficient supply coherence is avoided, and the efficiency of the supply device is improved.