- Preparation method of bisacodyl
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The present invention provides the preparation method shown in formula I., the preparation method of bisacodyl. The present invention provides a new method for the preparation of bisacodyl.
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- Preparation method of sodium picosulfate
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The invention belongs to the technical field of medicines, and relates to a preparation method of sodium picosulfate, in particular to condensation of pyridine -2 - formaldehyde and phenol under an acidic condition, and the obtained intermediate 4,4 ' - (2 - pyridinmethylene) - bisphenol uses sulfamic acid as a sulfonating agent. The method is relatively simple in process operation and high in sample purity.
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Paragraph 0040-0042; 0045-0047; 0050-0052; 0055-0057; ...
(2021/09/15)
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- Method for preparing high-purity sodium picosulfate intermediate and sodium picosulfate
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The invention discloses a method for preparing high-purity sodium picosulfate and an intermediate thereof. The method comprises the following steps: (1) dropwise adding concentrated sulfuric acid and 2-pyridylaldehyde into an acetonitrile solution of phenol in sequence for reaction; (2) adjusting to be alkaline after reaction quenching, neutralizing, dispersing and crystallizing, and refining a crude product by using organic alcohol; (3) adding the intermediate into a pyridine solution of chlorosulfonic acid, washing off pyridine by using acetone after the reaction is finished, treating into sodium salt by using an alkali, concentrating until dryness, extracting by using hot methanol, adding ethyl acetate for crystallization, filtering and drying to obtain a sodium picosulfate crude product; and (4) thermally extracting the crude product with absolute ethyl alcohol, adding a proper amount of purified water, cooling and crystallizing to obtain the sodium picosulfate monohydrate. According to the method, the high-purity intermediate and the sodium picosulfate monohydrate can be stably obtained by controlling the content of the isomer in the intermediate.
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Paragraph 0004; 0043-0057
(2021/05/29)
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- Colloidal gold detection kit for sodium picosulfate, bisacodyl and deacetylated bisacodyl and application of colloidal gold detection kit
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The invention discloses a novel compound. By adopting the compound, the recognition sensitivity and specificity of sodium picosulfate, bisacodyl and deacetylated bisacodyl can be improved. A chromatographic immune colloidal gold principle is applied, the compounds are made into antigens, a detection device is further formed, the detection device comprises a test strip and a reaction cup, and a detection line and a quality control line in the test strip are used for semi-quantitative detection of the content of sodium picosulfate, bisacodyl and deacetylated bisacodyl in a sample through line colorimetry. According to the invention, whether a sample contains sodium picosulfate, bisacodyl and deacetylated bisacodyl or not can be rapidly and accurately detected within a short time, the detection requirement of illegally adding sodium picosulfate, bisacodyl and deacetylated bisacodyl in weight-losing products can be met, and the requirement of on-site supervision and law enforcement of supervision departments and detection institutions can be met. Compared with the prior art, the kit has the characteristics of convenience in use, economy, quickness, easiness in manufacturing and low cost.
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Paragraph 0059-0060
(2021/05/26)
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- Synthesis method of sodium picosulfate
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The method comprises the following steps: adding acridine to an organic solvent, adding basic substances for reaction, adjusting pH values, filtering to obtain 4 and 4' - (2 -pyridylmethyl) bisphenol. 4, 4' - (2 - Picoline) bisphenol was added to the reaction solvent, a basic substance was added, and then a sulfonating reagent was added for the reaction. After the completion of the reaction, the crude product is obtained by quenching, extraction, concentration and recrystallization. The crude product was recrystallized from sodium sulfate to give a qualified sodium sulfate product. The method has the advantages that the process route is simple, the operation is simpler, the yield is increased and the like, the purity of the intermediate produced by the method is high, and the sodium metabisulfite meeting the requirements of the pharmacopeia can be easily obtained to solve the defects caused by the prior art.
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Paragraph 0055-0058; 0061-0064; 0067-0070
(2021/09/08)
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- Preparation and application of broad-spectrum antibody for simultaneously detecting three illegal additives in weight-losing health food
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The invention discloses a preparation method and application of a broad-spectrum antibody for simultaneous detection. The invention firstly provides two haptens, namely a hapten 1 and a hapten 2, wherein the structural formula of the hapten 1 is shown as a formula (I); and the structural formula of the hapten 2 is shown as a formula (III). According to the present invention, the hapten 1 is used to prepare the antibody for simultaneously detecting the three illegal additives in the weight-losing health food, the hapten 2 is used to prepare an artificial antigen 2 for coating, and the antibody has high sensitivity and high specificity on the three illegal additives in the weight-losing health food so as to meet the detection limit required by market supervision; meanwhile, an immunoassay method which is low in cost, high in sensitivity and stable and is used for simultaneously detecting three illegal additives in the weight-losing health-care food is established, and the immunoassay method has a good application prospect.
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Paragraph 0059; 0069-0071; 0088-0091
(2021/08/28)
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- Pegylated triarylmethanes: Synthesis, antimicrobial activity, anti-proliferative behavior and in silico studies
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We describe herein the synthesis, characterization and biological studies of novel PEGylated triarylmethanes. Non-symmetrical and symmetrical triarylmethanes series have been synthesized by Friedel-Crafts hydroxyalkylation or directly from bisacodyl respectively followed by a functionalization with PEG fragments in order to increase bioavailability and biological effectiveness. The antimicrobial activity was investigated against Gram-positive and Gram-negative foodborne pathogens and against Candida albicans, an opportunistic pathogenic yeast. The anti-biocidal activity was also studied using Staphylococcus aureus as a reference bacterium. Almost all PEGylated molecules displayed an antifungal activity comparable with fusidic acid with MIC values ranging from 6.25 to 50 μg/mL. Compounds also revealed a promising antibiofilm activity with biofilm eradication percentages values above 80% for the best molecules (compounds 4d and 7). Compounds 7 and 8b showed a modest antiproliferative activity against human colorectal cancer cell lines HT-29. Finally, in silico molecular docking studies revealed DHFR and DNA gyrase B as potential anti-bacterial targets and in silico predictions of ADME suggested adequate drug-likeness profiles for the synthetized triarylmethanes.
- Abdmouleh, Fatma,Ali, Mamdouh Ben,Arbi, Mehdi El,Ferroud, Clotilde,Goya-Jorge, Elizabeth,Guenineche, Léna,Lagarde, Nathalie,Liagre, Bertrand,Martin, Frédérique,Ricco, Christophe,Riccobono, Charlotte,Veitía, Maité Sylla-Iyarreta
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- Hapten BIS for rapidly detecting bisacodin, artificial antigen, antibody of artificial antigen and detection method
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The invention discloses a hapten BIS for rapidly detecting bisacodin, an artificial antigen, an antibody of the artificial antigen and a detection method. The invention firstly provides a hapten BIS for detecting bisacodin, and the structural formula of the hapten BIS is shown as a formula (I): an artificial antigen and an antibody for detecting bisacodin are prepared by using the hapten, the antibody has high sensitivity and high specificity recognition capability compared with bisacodin, the detection range of the antibody is 0.09-4.92 mu g/kg, and the lowest detection limit is 0.07 mu g/kg.Therefore, the bisacodin antibody prepared by the invention is high in detection sensitivity and strong in specificity in comparison with sacodin, and can meet the field detection requirements of large-batch samples; in addition, the hapten BIS, the artificial antigen and the antibody are simple in preparation method and low in cost, and have wide application prospects in detection of bisacodin.
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Paragraph 0035; 0041-0043; 0046-0048; 0051-0053
(2021/01/15)
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- Light-induced metal-free transformations of unactivated pyridotriazoles
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A highly efficient and practical method for incorporation of the arylmethylpyridyl moiety into diverse molecules has been developed. This method features the transition metal-free light-induced room temperature transformation of pyridotriazoles into pyridyl carbenes, which are capable of smooth arylation, X-H insertion, and cyclopropanation reactions. The synthetic usefulness of the developed method was illustrated in a facile synthesis of biologically active molecules.
- Zhang, Ziyan,Yadagiri, Dongari,Gevorgyan, Vladimir
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p. 8399 - 8404
(2019/09/30)
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- A process for preparing sodium new method (by machine translation)
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The invention relates to a method for preparing (V) indicated by the sodium of the method, the method comprises the following steps: (a) in formula (I) indicated by the 2 - picolinic ester as the starting material, as shown in formula (II) of 4 - halogenated phenyl ether in the formula (III) Grignard reaction indicated by the 4', 4" - dialkoxy diphenyl - (2 - pyridine) - methanol (compound III). (B) 4 ', 4 "- dialkoxy diphenyl - (2 - pyridine) - methanol (compound III) in the Lewis acid under the action of removing a water molecule and alkoxy alkyl, formula (IV) as shown by a 4', 4" - dihydroxy phenyl - (2 - pyridine) - methane (compound IV). (C) 4', 4" - dihydroxy phenyl - (2 - pyridine) - methane with chlorosulfuric acid in sulfuric acid esterification reaction, sodium hydroxide after treatment, to obtain crude sodium, by recrystallization to obtain high-purity sodium (compound V). The present invention provides a kind of existing technology with the different sodium new preparation method, the method is simple in operation, the atom economy is high, is suitable for industrial production. (by machine translation)
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- Synthetic method of 4,4'-(2-pyridylmethylene)diphenol diacetate
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The invention discloses a synthetic method of 4,4'-(2-pyridylmethylene)diphenol diacetate. The preparation method comprises the steps of adding solvent ethyl acetate or dichloroethane alpha-dextrin into raw material phenol, slowly dropwise adding sulfuric acid and 2-pyridylaldehyde while cooling, after the dropwise adding is finished, stopping reaction, adding ethanol for dissolving while cooling,dropwise adding the reactant into a 20% sodium carbonate solution so as to separate out white solids, filtering, washing to obtain an intermediate compound, purifying and drying the intermediate compound, carrying out reflux on the intermediate compound and acetic anhydrideor for 2-4 hours under the effect of anhydrous sodium acetate, and after the reaction is finished, carrying out elutriation,filtration, washing with water, ethanol decolorization and recrystallization, so as to obtain white powder, namely the target compound 4,4'-(2-pyridylmethylene)diphenol diacetate. The preparation method is simple and high in product quality and yield, and the raw materials are easily available.
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Paragraph 0013; 0025-0027; 0029-0031; 0033-0035
(2018/11/22)
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- STABILIZED LIQUID FORMULATIONS CONTAINING PICOSULFATE
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Stable liquid formulations containing picosulfate and magnesium citrate are provided. The formulations are useful to treat constipation or for the clearance of the bowel prior to X-ray examination, endoscopy or surgery.
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Page/Page column 43-45
(2018/09/25)
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- A process for preparing sodium method
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The invention discloses a method for preparing sodium picosulfate, which comprises the following steps: 1) preparing a 2-chlorophenol-ethanedioic acid mixture M and a 2-pyridylaldehyde-concentrated sulfuric acid mixture N; 2) dropwisely adding the mixture M obtained in the step (1) into the mixture N at 0-10 DEG C, continuing reaction at 20-30 DEG C, regulating the pH value to 8 with a sodium hydroxide solution, carrying out vacuum filtration, and washing with water to obtain a 3,3'-dichloro-4,4'-(pyridyl-2-yl-methylene)biphenol crude product; 3) dissolving the crude product in a 4M sodium hydroxide solution, adding a nickel aluminum alloy, stirring to react, filtering to take the filtrate, regulating the pH value with 10% acetic acid, filtering, washing with water, recrystallizing with methanol, filtering, and carrying out vacuum drying to obtain 4,4'-(pyridyl-2-yl-methylene)biphenol; and 4) dissolving the 4,4'-(pyridyl-2-yl-methylene)biphenol in pyridine, dropwisely adding chlorosulfonic acid at 0-10 DEG C to react, quenching with ice water, regulating the pH value with a sodium hydroxide solution, extracting with dichloromethane, concentrating the water phase under reduced pressure, recrystallizing with methanol, filtering, and carrying out vacuum drying. The method has the advantages of higher sodium picosulfate yield and fewer byproducts.
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Paragraph 0054; 0058
(2017/08/31)
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- Method for preparing high-purity sodium picosulfate
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The invention belongs to the field of medicine chemical engineering, particularly to a method for preparing high-purity sodium picosulfate. The method mainly comprises the following steps: condensing 2-pyridylaldehyde (a compound 2) and phenol (a compound 3) to obtain 4',4''-dihydroxy diphenyl-(2-pyridine)-methane (a compound 4) and ortho-isomeride 2',4''-dihydroxy diphenyl-(2-pyridine)-methane (a compound 5), dissolving the compound 4 and the compound 5 with water/furanidine, adjusting the pH to 8.0-8.5, adding ammonium ferrous sulfate until the solution is light blue, then adjusting the pH value to 6.5-7.0, dissolving out plenty of solid, conducting suction filtration to separate the high purity compound 4, and further synthesizing sodium picosulfate.
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Paragraph 0028; 0029; 0030; 0031
(2016/11/21)
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- Sodium picosulfate intermediate and sodium picosulfate preparation method
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The invention provides a sodium picosulfate intermediate preparation method. The sodium picosulfate intermediate preparation method is characterized by comprising the steps that 2-pyridylaldehyde and phenol are used as raw materials, trichloromethane is used as a solvent, and reaction liquid is formed after even mixing; acid substance is dropwise added to the reaction liquid, the solutes 2-pyridylaldehyde and phenol in the reaction liquid complete chemical reaction in an acidic environment to prepare a solution containing an intermediate; crystallization and purification are conducted on the solution to obtain a sodium picosulfate intermediate, namely 4,4'-(2- pyridine methylene)-phenol. According to the preparation method of the intermediate, the invention further provides a sodium picosulfate preparation method. Based on the methods provided by the invention, the isomer content of the intermediate in the synthesis process is reduced, the purity, conversion rate and reaction rate of the intermediate are improved, and meanwhile the yield is improved remarkably.
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Paragraph 0062; 0063
(2018/02/04)
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- Synthesis of triphenylmethane derivative: Bisacodyl
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A new method for the synthesis of bisacodyl 1 is described. The key step involves migration of 2-pyridacyl group of phenyl pyridine-2-carboxylate 4 in AlCl3 at 160 °C to yield the intermediate 4-hydroxyphenyl (2-pyridyl) ketone 5a. The reaction of 5a with phenol using H3PO 4 gives 1. This method has advantage over the existing literature methods because easily available pyridine-2-carboxylic acid is used as a starting material instead of the less stable pyridine-2-carboxaldehyde.
- Mereyala, Hari Babu,Sambaru, Kalyani
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p. 615 - 617
(2007/10/03)
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