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Analysis

1.117487763Rapid detection method for toluenesulfobutyl urea in marine functional food
CN 02.02.2024
Int.Class C12N 5/20
CCHEMISTRY; METALLURGY
12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
NMICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
5Undifferentiated human, animal or plant cells, e.g. cell lines; Tissues; Cultivation or maintenance thereof; Culture media therefor
10Cells modified by introduction of foreign genetic material, e.g. virus-transformed cells
12Fused cells, e.g. hybridomas
16Animal cells
18Murine cells, e.g. mouse cells
20one of the fusion partners being a B lymphocyte
Appl.No 202311291969.4 Applicant SERICULTURE & AGRI-FOOD RESEARCH INSTITUTE GAAS Inventor ZHOU SHENGYANG
The invention discloses a rapid detection method for toluenesulfonediamide in marine functional food, and belongs to the technical field of food safety immunodetection. The invention discloses a method for rapidly detecting toluenesulfobulurea in marine functional food, which comprises the following steps: reacting methyl 4-sulfonylbenzoate with n-butyl isocyanate to prepare a hapten of toluenesulfobulurea, coupling the hapten with carrier protein to obtain an artificial antigen for immunization, obtaining a monoclonal antibody by applying an artificial antigen sieve, and detecting the content of toluenesulfobulurea in marine functional food. The antibody has high sensitivity and high specificity to toluenesulfonediamide. And a detection method of the toluenesulfourea colloidal gold immunochromatography test strip is established by utilizing the toluenesulfourea antibody, so that the content of the toluenesulfourea illegally added in the marine health food can be rapidly detected, a core material is provided for establishing an immunochromatography detection method of the toluenesulfourea, and the method has a practical application value. The synthesis steps are simple and effective, and the method can be completely used in immunoassay.
2.102557997Preparation method of p-toluenesulfonylurea
CN 11.07.2012
Int.Class C07C 311/58
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
311Amides of sulfonic acids, i.e. compounds having singly-bound oxygen atoms of sulfo groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
50Compounds containing any of the groups X being a hetero atom, Y being any atom
52Y being a hetero atom
54either X or Y, but not both, being nitrogen atoms, e.g. N-sulfonylurea
57having sulfur atoms of the sulfonylurea groups bound to carbon atoms of six-membered aromatic rings
58having nitrogen atoms of the sulfonylurea groups bound to hydrogen atoms or to acyclic carbon atoms
Appl.No 201210012306.X Applicant Jinan IFT Science & Technology Co., Ltd. Inventor Yue Tao
The invention discloses a preparation method of p-toluenesulfonylurea. The preparation method adopts 4-toluenesulfonamide, inorganic base and urea as raw materials and comprises the following steps of: firstly lead the 4-toluenesulfonamide and the inorganic base to react in an organic solvent, obtaining p-toluenesulfonyl sodium, then adding urea to react with the p-toluenesulfonyl sodium, obtaining the p-toluenesulfonyl sodium, then acidifying the obtained p-toluenesulfonyl sodium, and obtaining a crude p-toluenesulfonylurea product, further purifying the crude product to obtain the p-toluenesulfonylurea, wherein the molar ratio of the 4-toluenesulfonamide, inorganic base and urea is 1:1.02-1.5:1-1.9. The preparation method has the advantages of simple process, high utilization ratio of raw materials, less environmental pollution, low production energy consumption, high product yield, short reaction period, and low production cost; and the prepared product can be used as the intermediate and is suitable for industrial production.
3.339699The manufacture of aromatic amino-aldehyde compounds
GB 18.12.1930
Int.Class Appl.No 2898629 Applicant IG FARBENINDUSTRIE AG Inventor
339,699. Carpmael, A., (I. G. Farbenindustrie Akt.-Ges.). Sept. 24, 1929. Aromatic aminoaldehyde compounds are manufactured by heating aldehydes of the benzene and anthraquinone series containing easily .replaceable halogen atoms with acid amides or sulphonamides or their monoalkyl-, aralkyl-, or aryl-derivatives in the presence of an acid binding agent, with or without the addition of a diluent and of a catalyst, and saponifying. the acidylamino- or sulphamino-compounds obtained. In examples, (1) 5-nitro-2-chlorbenzylaldehyde is heated with p - toluenesulphonamide, potassium carbonate, copper powder and cuprous chloride with or without nitrobenzene to give 5-nitro-2-p-toluenesulphaminobenzaldehyde; with benzamide to give 5- nitro-2-benzoylamino- and with phthalimide to give 5-nitro-2-phthaliminobenzaldehyde; these are saponified to 5-nitro-2-aminobenzaldehyde; (2) ochlorobenzaldehyde similarly with p - toluenesulphonamide yields 2-p-toluenesulphaminobenzaldehyde, whilst p-chlorobenzaldehyde and its 3- nitro-derivative yield the corresponding aminoaldehydes; by heating o-chlorobenzaldehyde with p-toluenesulpho-p-toluidide and saponifying, 6- methylacridine results: (3) 2 : 6-dichlorobenzaldehyde with p-toluenesulphonamide yields, according to the proportions of the reagents, 2-p-toluenesulphamino-6-chlorobanzaldehyde or 2 : 6-di-ptoluenesulphaminobenzaldehyde, and on saponification 6-chloro-2-amino. or 2:6-diaminobenzaldehyde; (4) 3-nitro-2 : 6-dichlorobenzaldehyda with p-toluenesulphonamide in nitrobenzene solution yields 3-nitro-2 : 6-di-p-toluenesulphonaminobenzaldehyde and on saponification 3-nitro-2 : 6- diaminobenzaldehyde; (5) 2 : 5 - dichloroterephthalaldehyde with p-toluenesulphonamide yields 2 : 5 - di - p - toluenesulphaminoterephthalaldehyde and on saponification 2 : 5-diaminoterephthalaldehyde; (6) 1-chloroanthraquinone-2-aldehyde with p-toluenesulphonamide using potassium acetate as binding agent in amyl alcohol solution yields on saponification 1-aminoanthraquinone-2- aldehyde. Specifications 16272/10 and 214,765 are referred to. The Provisional Specification refers also to aldehydes of the naphthalene and anthracene series.
4.636737Toluenesulphonates and their method of preparation
GB 03.05.1950
Int.Class C07C 391/02
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
391Compounds containing selenium
02having selenium atoms bound to carbon atoms of six-membered aromatic rings
Appl.No 3774546 Applicant GEN ANILINE & FILM CORP Inventor
Toluenesulphonates of the general formula CH3-C6H4-SO3(CH2)m-Se-R, where R is a phenyl or naphthyl radical and m is 2 or 3, are prepared by treating a toluenesulphonyl chloride with an alcohol of the formula R-Se-(CH2)m-OH, preferably in the presence of a base. Examples are given of the preparation of (1) b -phenylselenoethyl p-toluenesulphonate from b -phenylselenoethyl alcohol and p-toluenesulphonyl chloride in presence of pyridine, and (2) a -phenylselenopropyl p-toluenesulphonate from a -phenylselenopropyl alcohol and p-toluenesulphonyl chloride in presence of pyridine. The preparation of the corresponding o- and m-toluenesulphonates is referred to. Specification 636,738, [Group IV (c)], is referred to. The Specification as open to inspection under Sect. 91 comprises also the preparation of analogous compounds wherein the selenium is replaced by oxygen or sulphur and includes examples of the preparation of p-(tert.-butyl)-phenoxyethyl p-toluenesulphonate, di-iso-butyl-phenoxyethyl, p-toluenesulphonate, p-cyclohexylphenoxyethyl, p-toluenesulphonate, p-chlorophenoxyethyl, p-toluenesulphonate, p-phenylphenoxyethyl, p-toluenesulphonate, b -phenylthioethyl, p-toluenesulphonate, phenylthiopropyl, p-toluenesulphonate, p-chlorophenoxypropyl, p-toluenesulphonate, p-(tert.-butyl) - phenoxyethyl o - (and m-) - toluenesulphonates, and phenylthioethyl o-toluenesulphonate. This subject-matter does not appear in the Specification as accepted.
5.1255701PROCESS FOR PRODUCING MONOTERTIARY BUTYL TOLUENEDIAMINE
CA 13.06.1989
Int.Class C07C 209/68
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
209Preparation of compounds containing amino groups bound to a carbon skeleton
68from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
Appl.No 508964 Applicant Inventor BURGOYNE, WILLIAM F., JR.
PATENT 174-P-USO3210 ABSTRACT This invention pertains to a process for selectively reactingisobutylene with toluenediamine to form monotertiary butyl toluenediamineat high conversion. The process comprises contacting a toluenediaminefeedstock containing the 2,4- or 2.6-toluenediamine isomer withisobutylene or an isobutylene precursor in the presence of an acidiczeolite catalyst having an effective pore size of about 6 to 8Angstroms. An H-Y zeolite is preferred.
6.593518Manufacture of derivatives of p-toluene-sulphonamide
GB 20.10.1947
Int.Class C07C 311/37
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
311Amides of sulfonic acids, i.e. compounds having singly-bound oxygen atoms of sulfo groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
30Sulfonamides, the carbon skeleton of the acid part being further substituted by singly-bound nitrogen atoms, not being part of nitro or nitroso groups
37having the sulfur atom of at least one of the sulfonamide groups bound to a carbon atom of a six-membered aromatic ring
Appl.No 51845 Applicant BRITISH SCHERING RES LAB LTD Inventor
p-Toluene sulphonamide derivatives of the general formula wherein X represents -NH2OC-CH2NH2 are obtained by condensing in solution in a water-miscible organic solvent (a) a p-acetamido-benzene sulphonyl halide or an o -acetamido-p-toluene sulphonyl halide with o -amino-p-toluene sulphonamide, followed by hydrolysis of the acetyl group; (b) a p-nitrobenzene sulphonyl halide or an o -nitro-p-toluenesulphonyl halide with o -amino-p-toluenesulphonamide, followed by reduction of the nitro group. The condensations are preferably effected in solution in aqueous acetone, but other water-miscible solvents, e.g. methyl ethyl ketone or dioxane may be used. The condensation may be carried out in the presence of sodium bicarbonate. In examples: (1) o -amino-p-toluenesulphonamide and p-acetamidobenzenesulphonyl chloride, in aqueous acetone are treated with sodium bicarbonate and water, the precipitated o - (p - acetamidobenzenesul - phonamido) - p - toluenesulphonamide being hydrolysed with 5N hydrochloric acid and the reaction mixture neutralized to isolate o -(p-aminobenzenesulphonamido)-p-toluenesulphonamide; (2) o - amino - p - toluenesulphonamide and p - nitrobenzenesulphonyl chloride are treated as in (1), and the precipitated o -(p-nitrobenzenesulphonamido)-p-toluene sulphonamide is reduced in aqueous methylated spirit with concentrated hydrochloric acid and iron powder, prior to adding ammonia and extracting the residue with alcohol to obtain the product of (1); (3) o -acetamido-p-toluenesulphonyl chloride and o -amino-p-toluenesulphonamide are treated as in (1), and the precipitated o -(o 1-acetamido-p-toluenesulphonamido) -p-toluenesulphonamide is hydrolysed by boiling with alcoholic 10 per cent hydrochloric acid, ammonia being added to precipitate the corresponding amino compound.
7.117865859Preparation method of enantiomerically pure p-toluenesulfonamide
CN 12.04.2024
Int.Class C07C 313/06
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
313Sulfinic acids; Sulfenic acids; Halides, esters or anhydrides thereof; Amides of sulfinic or sulfenic acids, i.e. compounds having singly-bound oxygen atoms of sulfinic or sulfenic groups replaced by nitrogen atoms, not being part of nitro or nitroso groups
02Sulfinic acids; Derivatives thereof
06Sulfinamides
Appl.No 202211670042.7 Applicant CHANGZHOU QINUO BIOLOGICAL TECHNOLOGY CO., LTD. Inventor FENG HONGFENG
The invention discloses a preparation method of enantiomerically pure p-toluene sulfinamide, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking sodium p-toluenesulfinate as a raw material, firstly reacting with thionyl chloride to generate acyl chloride, then reacting with ammonia water to generate p-toluenesulfinamide, then reacting with acid anhydride under the action of strong base to obtain N-(ethyl or benzyl) acyl p-toluenesulfonamide, and then splitting and dissociating with chiral 1, 2-dimethyl cyclohexanediamine to obtain corresponding chiral N-(ethyl or benzyl) acyl p-toluenesulfonamide. Then carrying out deprotection in sulfuric acid/methanol or oxalyl chloride/DMF (Dimethyl Formamide) to generate a Vilsmeier reagent, and then reacting with hydrazine hydrate to obtain the enantiomerically pure p-toluenesulfonamide. The route has the advantages of easily available raw materials, low cost, coherent operation, low requirement on equipment, and recyclable resolving agent, and is suitable for industrial large-scale production.
8.112079753Production process of p-toluenesulfonamide urea
CN 15.12.2020
Int.Class C07C 303/36
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
303Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
36of amides of sulfonic acids
Appl.No 202010957735.9 Applicant JIAXING JINLI CHEMICAL CO., LTD. Inventor ZHU JIANHUA
The invention discloses a production process of p-toluenesulfonamide urea, and the process comprises the following steps: S1, adding ammonium sulfite into a reaction kettle, dissolving the ammonium sulfite in 3-5 times of water, then adding sodium hydroxide and dissolving sodium hydroxide, adding p-toluenesulfonyl chloride, reducing p-toluenesulfonyl chloride into p-toluenesulfinate, and acquiringa p-toluenesulfinate aqueous solution; S2, adding azodicarbonamide into the p-toluenesulfinate aqueous solution obtained in the step S1, carrying out a reaction, and stopping the reaction when no gasis discharged; performing cooling, filtering, washing and drying to obtain the target product p-toluenesulfonamide urea. The production process of p-toluenesulfonamide urea is simple in steps and convenient for automatic continuous production; only water is used as a solvent, no organic solvent is used, and safety and environmental friendliness are achieved; the yield is high and reaches 95% or above, operation is easy, raw materials are easy to obtain, and the price is low; the process is a synthetic route suitable for large-scale automatic continuous production.
9.101650304Method for determining content of sodium p-toluenesulfinate in reduction process of p-toluenesulfonyl chloride
CN 17.02.2010
Int.Class G01N 21/33
GPHYSICS
01MEASURING; TESTING
NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
21Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
17Systems in which incident light is modified in accordance with the properties of the material investigated
25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
33using ultraviolet light
Appl.No 200910100908.9 Applicant Jiaxing University Inventor Wu Jianyi
The invention relates to a method for determining the content of sodium p-toluenesulfinate in a reduction process of p-toluenesulfonyl chloride. A wavelength of 282 nm, which does not absorb sodium 4-toluenesulfonate and absorbs a great amount of sodium p-toluenesulfinate, is obtained by respectively scanning ultraviolet-spectrum full wavelengths of standard solutions of the sodium 4-toluenesulfonate and the sodium p-toluenesulfinate, not only can favorably determine the content of the sodium p-toluenesulfinate, but also can satisfy the needs on detection sensitivity. Under the wavelength, the method not only can differentiate the sodium 4-toluenesulfonate from the sodium p-toluenesulfinate which are contained in the solution, but also can simultaneously achieve the quantitative determination of the sodium p-toluenesulfinate.
10.106938977Method for preparing p-toluenesulfonylhydrazide
CN 11.07.2017
Int.Class C07C 303/40
CCHEMISTRY; METALLURGY
07ORGANIC CHEMISTRY
CACYCLIC OR CARBOCYCLIC COMPOUNDS
303Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
36of amides of sulfonic acids
40by reactions not involving the formation of sulfonamide groups
Appl.No 102017000303582 Applicant LI BOQIANG Inventor LI BOQIANG
The invention provides a method for preparing p-toluenesulfonylhydrazide. The preparation method comprises that p-toluenesulfonamide, acetone azine and water as raw materials undergo a reaction to produce p-toluenesulfonylhydrazide at a certain temperature, after the reaction is finished, the precipitated solids are centrifuged and filtered, and the filter cake is washed and dried to form the p-toluenesulfonylhydrazide product. The method has the advantages of simple process, high reaction yield, high purity and few impurities of the product. The recovered ammonia and acetone as by-products can be used for synthesis of acetone azine, and the filtrate containing acetone azine and p-toluenesulfonamide can be directly used for preparing p-toluenesulfonylhydrazine. The method has a high raw material utilization rate and realizes a low production cost. The method is free of benzene as a solvent, does not produce corrosive hydrogen chloride gas and hydrochloric acid, has low equipment requirements, discharges less waste and is an environment-friendly production process.