73 results about "Methiodide" patented technology

The present invention relates to flavor oils including mint-, fruit- and spice-type flavors that are specially processed to substantially eliminate low-molecular weight sulfur compounds, in particular dimethyl sulfoxide (DMSO), which has been found to be the main precursor of malodorous species such as dimethyl sulfide and methyl mercaptan. These malodorous species are produced via oxidation-reduction reactions involving such sulfur-containing compounds present in flavor oils. A preferred processing method is an aqueous-washing process, which has advantages of being simple, inexpensive and easy to implement while importantly avoiding the problems of typical processes including non-selective removal of desirable components and subjecting the flavor oils to extreme conditions that may destroy other components and result in undesirable changes in flavor or odor character. Other processing methods to selectively remove non-desired components include (1) distillation to remove polar low boiling point components, (2) filtration through adsorbents selective for sulfur compounds, (3) countercurrent extraction and (4) column chromatography. The processing methods may optionally be followed by reengineering to add back desired components that may have been removed or altered during the processing. The specially processed flavor oils are particularly useful in oral care compositions comprising components with chemical reducing capability such as stannous ions, which react with the sulfur-containing compounds to produce malodorous products.

The invention discloses a synthesis method of taxane drug 7, 10-methoxy-docetaxel. The synthesis method includes using 7, 10-trichloro-ethoxycarbonyl-10-deacetylbaccatin III (compound 1, CAS (chemical abstracts service) number 95603-44-4) as starting material, using triethyl silicon substrate for protection, and performing reactions of removal of protecting group of trichloro-ethoxycarbonyl, dimethyl sulfide etherification, hydrogenation reduction, removal of protecting group of the triethyl silicon substrate, side chain condensation and side chain deprotection to obtain the 7, 10-methoxy-docetaxelf with more than 99% purity. Reaction conditions are simple and mild. The synthesis method has the advantages that the required equipment is simple and is easy to operate, and methylate reagents such as highly toxic methyl iodide or dimethyl sulfate is not needed. The synthesis method is applicable to industrial production.

The invention relates to the field of organic synthetic chemistry and specifically relates to a synthetic method of tulathromycin. No Cbz (carbamazepine)-Cl protection is used in the synthetic method of tulathromycin, which is provided by the invention; no Pd / C-H2 system needs to be used for deprotection; therefore, the operation is safer; besides, the reaction does not need to be carried out at an ultralow temperature, so that the energy source is saved; moreover, dimethylsulfide generated in the reaction process can be recovered and reused, so that the cost is relatively low; the reaction only comprises three steps, which is simpler than that in the known documents.

The invention discloses a method for preparing an intermediate of flutriafol bactericide, which comprises the following three steps: a first step, that is, dimethyl sulphide and dimethyl sulfate react in organic solvent to generate onium salt; a second step, that is, fluorobenzene and o-fluorobenzene formyl chloride are subjected to Friedel-Crafts reaction to generate 2, 4-difluoro diphenyl ketone; and a third step, that is, the 2, 4-difluoro diphenyl ketone and the onium salt react under alkaline condition to obtain the intermediate of flutriafol with high content. The method effectively controls the content of impurities in the intermediate of the flutriafol below 0.5 percent.

The invention relates to the technical field of preparation of dimethyl disulfide and provides a production method of dimethyl disulfide. The production method includes the steps of A, using sodium hydroxide solution containing catalyst to absorb a methyl mercaptan mixture so as to obtain mixed solution containing sodium thiomethoxide; B, mixing oxygen or oxygen-rich air with the alkaline solution obtained in the step A, allowing reaction to generate dimethyl disulfide, dimethyl sulfide and sodium hydroxide; and C, separating the oxygen or oxygen-rich air surplus in the reaction to generate dimethyl sulfide so as to obtain dimethyl disulfide liquid. The production method has low cost, high yield and low pollution. A production apparatus of dimethyl disulfide is further provided; the production apparatus comprises an absorption column, a heater, an oxidization column, a flash separator tank and a recovery system connected in order through a pipeline, wherein the heater is used for heating the alkaline solution to a set temperature, the oxidization column is used for generating dimethyl disulfide, the flash separator tank is used for separating materials, and the recovery system is used for recovering the alkaline solution. The production apparatus is automatically controllable, thus labor is saved, reutilization of the alkaline solution is achieved and production cost is lowered.

A method for preparing a fluralana intermediate, provided by the invention, comprises the following steps: carrying out nucleophilic addition reaction on 1-(3, 5-dichlorophenyl)-2, 2, 2-trifluoroethanone, carrying out acidolysis, reacting with a Grignard reagent, carrying out oxidation, carrying out oxidation cyclization reaction, reacting with hydroxyl(toluenesulfonyloxy)benzene iodide, and reacting with a trimethoxyphosphorus solution to finally generate the fluralan. In the preparation process, a catalyst and dimethoxy zinc are not needed, ultralow-temperature reaction conditions of -78 DEG C are not needed, operation is easy and convenient, meanwhile, reagents such as ozone and dimethyl sulfide which are harmful to the environment are replaced, and the method is more environmentally friendly. The invention also provides the intermediate for preparing the fluralan.

The invention discloses a method for simultaneously determining multiple thioether odor substances in a water body. The multiple thioether odor substances in the water body are simultaneously determined by utilizing headspace solid phase microextraction-gas chromatograph-mass spectrometer (HSPE-GC / MS). The method disclosed by the invention can be used for simultaneously determining common thioethers in various water bodies, such as dimethyl sulfide (DMS), dimethyl disulfide (DMDS), dimethyl trisulfide (DMTS), methyl ethyl sulfide (MES), diethyl sulfide (DES) and diethyl disulfide (DEDS). At present, reports about simultaneous determination of the multiple substances by adopting one method do not exist, the method fills the blank, multiple thioethers in the water body are quantitatively analyzed at a time, and the detection efficiency is greatly improved. The method is high in sensitivity and good in reproducibility, the detection limit of various thioether odor substances is below theodor threshold value of the odor substances, and the method can be widely applied to detection of dynamic changes of the various thioether odor substances in natural water.

The invention discloses a synthesis method of an aromatic vinyl trifluoromethylthio ether compound, and belongs to the technical field of chemical synthesis. According to the synthesis method disclosed by the invention, the aromatic vinyl trifluoromethylthio ether compound is prepared by taking trans-nitro aryl ethylene as a substrate, silver trifluoromethylthio as a thioether reagent and copper trifluoroacetic acid as a catalyst, and adding an oxidizing agent and an additive. Raw materials used by the method are easy to obtain, the reaction is simple to operate, the yield is high, and the substrate universality is good; the obtained aromatic vinyl trifluoromethylthio ether product has important application in the medicine, pesticide and function material fields.

The invention provides a new synthesis method of 9-boron bicyclo (3,3,1)-nonane (9-BBN). 1,5-cyclooctadiene and borane are taken as raw materials, a reaction is carried out in a tetrahydrofuran solvent, and the 9-boron bicyclo (3,3,1)-nonane (9-BBN) is synthesized while yield is as high as 98%. The new synthesis method comprises the following steps of adding a smashed 4A molecular sieve, tetrahydrofuran, 1,5-cyclooctadiene and zirconium tetrachloride into a reaction flask, stirring for 1 hour, dropwise adding a dimethyl sulfide complex of borane at the temperature about 0 DEG C, carrying out a reflux reaction for 4 hours after dropwise addition is completed to obtain a product, cooling the obtained product to 0 DEG C and preserving heat for 3 hours, and filtering to obtain a 9-boron bicyclo (3,3,1)-nonane (9-BBN) solid product. The new synthesis method of the 9-boron bicyclo (3,3,1)-nonane (9-BBN) has the advantages of high yield, low cost, high product purity, easy operation, is beneficial to industrialization and has a good application prospect.

The invention discloses a novel preparation method of ulipristal acetate key intermediate 3,3,20,20-double (ethylenedioxy group)-5 alpha, 17 alpha- dihydroxyl-11 bata-[4-(N,N- dimethyl amidogen)- phenyl]-19-norprogesterone-9(11)-alkene, namely 3,3- ethylenedioxy group-17 beta-cyangroup female steroid-5(10), 9(11) diene-17 alpha-alcohol is used as a raw material, through the protection of hydroxyl, the addition of Grignard reagent and cyangroup, and the protection of ketal, and the target compound is obtained finally through 1,4 addition of alpha, beta unsaturation epoxide under the catalysis of a system of cuprous halides and dimethyl sulfide. The raw materials used in the method are safe and reliable, reaction is easy to control, reaction yield and stereoselectivity are high, and the method is applicable for industrial production.

According to the photocatalysis device and the method for removing the malodorous gas by using the photocatalysis device, wherein the hydrophobic photocatalyst prepared by the invention is placed in the photocatalysis device provided by the invention, so that the removal of the sulfur-containing malodorous gas under high humidity is realized; the prepared photocatalyst can always keep good catalytic activity and stability, the photocatalytic device is simple in structure and convenient to operate, especially under high humidity, the catalytic removal efficiency of foul organic sulfur compoundsis high; for example, the removal rate of dimethyl sulfide can reach 100% by means of the photocatalysis device.

The invention discloses a method for removing an odor organic gas, which is applicable to 2-dimethyl sulfide organic gas, thioalcohol organic gas, and thiophenol organic gas. The method comprises the following steps of: preparing a solvent mixture comprising an alcohol, and preparing an inorganic metal salt mixture from the solvent mixture and an inorganic metal salt mixture at the mass ratio of 1:0.02-0.08; starting stirring and introducing the odor 2-dimethyl sulfide organic gas, the odor thioalcohol organic gas, and the odor thiophenol organic gas into a container with an absorption solution; when the solution is saturated by absorption, distilling the absorption solution for recycling, and supplementing the inorganic metal salt mixture for recycling. The method disclosed by the invention is simple to operate, low in requirements for running equipment, and good in odor removal effect for the odor 2-dimethyl sulfide organic gas, the odor thioalcohol organic gas, and the odor thiophenol organic gas. The use amount of the inorganic metal salt is less, the solvent can be recycled, and finally, the black and odorless inorganic metal salt waste can be dehydrated and subjected to deep landfill treatment.

The invention discloses a florfenicol midbody, a preparation method thereof and a preparation method of florfenicol, and belongs to the field of veterinary drug preparation. The invention provides the florfenicol midbody shown in a formula IV, wherein R1 is dimethyl sulfide or methylene sulphonyl or methyl sulphonyl, R2 is TBS- or TMS- or MOM- or THP-, R3 is shown in the description, and R4 is dichloroacetyl or benzoyl or t-butyloxycarboryl. The invention further provides a preparation of the florfenicol midbody shown in the formula IV and a preparation method of florfenicol. The obtained florfenicol is low in cost, simple in technology and high in yield, and the product chirality purity reaches up to 98%.

The invention relates to an efficient dye flocculant as well as a preparation method and an application thereof. The efficient dye flocculant is characterized being prepared from a polymer main chainPHAM (poly(hydroxymethyl acrylamide)), cationic polymeric side chain PDMC-COOH (polymethacryloxyethyltrimethyl ammonium chloride containing carboxyl at the tail end), anionic polymeric side chain precursor PtBMA-COOH (poly(tert-butylmethacrylate) containing carboxyl at the tail end), functional polymeric side chain precursor PNVF-COOH (poly(N-vinylformamide) containing carboxyl at the tail end), DMF (dimethylformamide) solvent, a catalyst, namely, NHS (N-hydroxysuccinimide), EDC.CH3I (1-ethyl-3-(3-dimethylaminopropyl)carbodiimide methiodide), potassium hydroxide and CDTAD (cyclohexanediamine tetraacetic acid dianhydride), and the efficient dye flocculant is used for treating dye wastewater and artistic coating wastewater drained in the dye synthesis or dyeing and finishing process. The efficient dye flocculant has the advantages of being high in trapping capability and settling speed, capable of treating complexing heavy metal ions, trapping dye molecules and complexing heavy metal ions in a few seconds and growing into large settling particles rapidly to achieve the purpose of rapid dye separation, simple to operate, low in treatment cost, high in adaptability and the like.

The invention belongs to the technical field of heterocyclic chemistry, particularly relates to a heterocyclic anti-tumor chemical medicine, and more particularly relates to a synthesis method of pyrimidine heterocyclic ring-containing antitumor medicine molecule AZD6738. A chiral ligand induced asymmetric oxidation method is used, chiral ligands are combined with cheap oxidizing agents (such as hydrogen peroxide) to oxidize dimethyl sulfide to prepare chiral sulfoxide, conversion of the chiral sulfoxide is efficiently achieved, a chiral sulfoxide compound 7 for the AZD6738 is prepared, and then the final product AZD6738 is prepared through an intermittent reaction. Besides, the AZD6738 is prepared by adopting a fluid chemical method, the total yield of total synthesis of the AZD6738 is remarkably improved compared with that of an intermittent reaction, and the method is suitable for industrial production.

The invention belongs to the technical field of synthesis of medicines and particularly relates to a nifuratel preparation method. The nifuratel preparation method comprises the following steps: taking epoxy propyl dimethyl sulfide as the starting material, having a ring-opening reaction with tert-butyl carbazate to obtain N'-(2-hydroxyl-3-methylmercapto-propyl)-tert-butyl carbazate; having a ringclosing reaction with urea under the catalytic action of cuprous bromide, obtaining a key intermediate N-(Boc-amino)-5-methylmercapto-methyl-2-oxazolidinone; hydrolyzing 5-nitro furfural diacetate under the action of trifluoroacetic acid to obtain 5-nitrofurfural, condensing with N-(Boc-amino)-5-methylmercapto-methyl-2-oxazolidinone, and obtaining nifuratel. In the process route, the cheap easy-to-get agents are chose, the operation difficulty and the processing burden caused after the reaction are reduced, the environmental harm is reduced, the production safety is guaranteed, and the preparation method is an easy, green and economical process route for the preparation of the nifuratel.

The invention provides a preparation method of o-aminothiophenol. The preparation method comprises the following steps: putting o-chloronitrobenzene into sodium methyl mercaptide, and performing heating under the action of a catalyst to carry out a methyl vulcanization reaction so as to prepare o-nitrophenyl dimethyl sulfide; putting o-nitrophenyl thioether into a solvent, and carrying out hydrogenation reduction to prepare o-aminobenzene thioether; and demethylating the o-aminothiophenol under the action of hydrobromic acid to obtain the o-aminothiophenol. The preparation method of o-aminothiophenol has the advantages of high yield and high product purity.

In one aspect, provided herein are methods for treating colorectal cancer in a human subject, the methods comprising administering to the human subject a composition comprising a mitogen-activated protein kinase kinase (MEK) inhibitor and a composition comprising bisphosphonate. In a particular aspect, provided herein is a method for treating colorectal cancer in a human subject, the method comprising administering to the human subject trametinib dimethyl sulfide or a composition thereof and zoledronic acid or a composition thereof.

The invention discloses a synthesis method of (R)-5-methylpyrrolidone-2-one. The synthesis method comprises following steps: step one, adding methyl levulinate, borane dimethyl sulfide, and a catalystinto a solvent, and carrying out reactions for 1 to 5 hours to obtain (R)-4-hydroxylmethyl pentanoate; step two, adding (R)-4-hydroxylmethyl pentanoate obtained in the step (1) into a reactor, introducing a nitrogen source and Raney nickel into the reactor, and carrying out catalytic reactions under a pressurized condition to obtain (R)-4-aminomethyl pentanoate; step three, adding (R)-4-aminomethyl pentanoate into a solvent, adding an alkaline catalyst, raising the temperature to 30-80 DEG C, and carrying out reactions for 0.5 to 5 hours to obtain the target product (R)-5-methylpyrrolidone-2-one; wherein the solvent in the step (1) is one or more of dichloromethane, toluene, dimethyl formamide, dimethyl sulfoxide, dichloromethane, and tetrahydrofuran. The synthesis method has the advantages of easily available and cheap raw materials, high atom utilization rate, high purity, easy purification, and high yield, and the chiral center does not need to be splitted.

The invention belongs to the technical field of sewage treatment, and particularly provides a novel deodorization process for high-standard control of sewage plant odor. A ''biotrickling-vacuum ultraviolet / catalysis'' combined process is adopted to realize efficient removal of low-concentration hydrogen sulfide, ammonia, methyl mercaptan and dimethyl sulfide in the sewage plant odor. The process is simple, low in cost and beneficial to industrial application.

The invention discloses a methyl mercaptan purification device which comprises a multi-stage condenser, an extraction tower, a coalescer, a degassing tower, a methyl mercaptan rectifying tower, a dimethyl sulfide rectifying tower, a wastewater rectifying tower and a dimethyl sulfide conversion reactor. The multistage condenser is connected with the methyl mercaptan synthesis reactor, a lower gas phase outlet is connected with the synthesis tail gas condenser, a bottom liquid phase outlet is connected with the lower part of the extraction tower, the extraction tower is connected with the coalescer and the condenser, a bottom discharge hole is connected with the middle part of the wastewater rectifying tower, the coalescer is connected with the extraction tower, the degassing tower and the methyl mercaptan rectifying tower, a top outlet of the methyl mercaptan rectifying tower is connected with the mercaptan storage tank, a bottom outlet is connected with a middle feed port of the dimethyl sulfide rectifying tower, the dimethyl sulfide rectifying tower is connected with the dimethyl sulfide conversion reactor, and a top outlet of the wastewater rectifying tower is connected with a tail gas washer. The device is reasonable in technological process, high in product methyl mercaptan purity, low in operation energy consumption and sufficient in dimethyl sulfide utilization, and is anideal methyl mercaptan purification device.

The invention relates to a novel chelating heavy metal capturing agent, and a synthesis method and application thereof. The technical scheme is characterized in that a polymer main chain polyhydroxyethyl acrylamide, a functional polymer side chain precursor polymer carboxyl-terminated poly(N-vinylformamide), water, a catalyst N-hydroxysuccinimide, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide methiodide, potassium hydroxide, ethylene glycol-bis(2-aminoethylether)-N,N,N',N'-tetraacetic acid dianhydride and carbon disulfide are employed for prepare the novel chelating heavy metal capturing agent, and the novel chelating heavy metal capturing agent is used to treat heavy metal wastewater discharged from electroplating, smelting, mining, beneficiation, chemical engineering and machinery. The functional group of the capturing agent can adsorb complexed heavy metal ions, and each basic unit can provide six coordination atoms for strong chelation and adsorption. Further, a chemical precipitation reaction between sodium dithiocarbamate at the side chain and a sedimentation aid is facilitated through a polymer brush, and a large aggregate is generated in seconds, so that rapid settling is realized and the operation is simple.

The invention discloses a heterogeneous photosensitizer based on a metal organic framework material as a carrier as well as a preparation method and application of the heterogeneous photosensitizer, and belongs to the technical field of preparation of environment-friendly functional composite materials. The heterogeneous photosensitizer disclosed by the invention is a metalloporphyrin@ZIF-8 composite material, wherein a metalloporphyrin compound which has strong absorption in a visible light region and can efficiently generate singlet oxygen (1O2) is loaded into a ZIF-8 metal organic framework material pore channel through a simple "one-pot" self-assembly method. Finally, the prepared heterogeneous photosensitizer is used for catalytic oxidation of thioanisole, then the catalyst can be recycled through simple centrifugation, washing and drying, and the heterogeneous photosensitizer is circularly used for catalytic oxidation of thioanisole and degradation of bisphenol A. The preparation method is simple, easy to operate, environmentally friendly, low in cost, good in repeatability and short in consumed time; the heterogeneous photosensitizer has strong absorption in a visible region, and 1O2 can be efficiently generated, so that thioether compounds can be selectively oxidized into sulfoxide under the condition of stirring at room temperature, the conversion rate is high, and the reusability is good.

Provided herein are compositions including oxotremorine (e.g., oxotremorine methiodide or Oxo-M) and 4-PPBP (e.g., 4-PPBP maleate). Also provided are methods of treating a connective tissue defect in a subject with oxotremorine and 4-PPBP. In addition, provided are scaffolds and methods of making same that include multiple fibers that include Oxo-M, 4-PPBP, and optionally icariin or kartogenin.

The invention discloses a novel preparation method of ulipristal acetate key intermediate 3,3,20,20-double (ethylenedioxy group)-5 alpha, 17 alpha- dihydroxyl-11 bata-[4-(N,N- dimethyl amidogen)- phenyl]-19-norprogesterone-9(11)-alkene, namely 3,3- ethylenedioxy group-17 beta-cyangroup female steroid-5(10), 9(11) diene-17 alpha-alcohol is used as a raw material, through the protection of hydroxyl, the addition of Grignard reagent and cyangroup, and the protection of ketal, and the target compound is obtained finally through 1,4 addition of alpha, beta unsaturation epoxide under the catalysis of a system of cuprous halides and dimethyl sulfide. The raw materials used in the method are safe and reliable, reaction is easy to control, reaction yield and stereoselectivity are high, and the method is applicable for industrial production.

The invention relates to a water-soluble binary chelic polymer molecular brush anionic dye catcher as well as a preparation method and application thereof. The water-soluble binary chelic polymer molecular brush anionic dye catcher is characterized by being prepared from polyhydroxyethyl acrylamide as a main chain of a polymer, carboxyl-containing poly(methacryloyloxyethyltrimethyl ammonium chloride) at the tail end of a cationic polymer side chain precursor polymer, carboxyl-containing poly(N-vinylformamide) at the tail end of a functional polymer side chain precursor polymer, water, a catalyst, namely N-hydroxysuccinimide, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide methiodide, potassium hydroxide and ethylene glycol bis(2-aminoethyl ether)-N,N,N',N'-tetraacetic acid and is applied totreatment of dye wastewater and artistic coating wastewater discharged in dye synthesis or dyeing and finishing processes. The water-soluble binary chelic polymer molecular brush anionic dye catcher has the advantages of high catching capacity, high sedimentation speed, simplicity and convenience in operation, low treatment cost, high adaptability and capability of treating complex heavy metal ions, catching anionic dye molecules and complex heavy metal ions within several seconds, realizing rapid growth to form large sedimented particles and achieving the aim of separating a dye.

The invention discloses a preparation method of nifuratel, which comprises the following steps: taking epoxypropyl dimethyl sulfide as an initial raw material, carrying out a synthetic reaction with carbon dioxide to obtain methylthio methyl ethylene carbonate, then carrying out a synthetic reaction with tert-butyl carbazate to obtain N-(tert-butyl formate-amino)-5-methylthio methyl-2-oxazolidinone, and finally, carrying out a reaction on the N-(tert-butyl formate-amino)-5-methylthio methyl-2-oxazolidinone and the N-(tert-butyl formate-amino)-5-methylthio methyl-2-oxazolidinone to obtain the nifuratel. And carrying out condensation reaction with 5-nitrofurfural to obtain nifuratel. The nifuratel prepared by the method is relatively high in yield and purity, the preparation process is green and pollution-free, meanwhile, the problem of carbon dioxide waste gas pollution is solved, and the defects of environmental pollution, potential safety hazards, raw material waste and the like existing in an existing nifuratel synthesis process are overcome.

The invention discloses a preparation method of a substituted benzo [B] naphthobenzene [2, 3-D] thiophene derivative, which comprises the following steps: reacting 2-naphthyl dimethyl sulfide serving as a raw material at low temperature to obtain an intermediate S-1, carrying out coupling reaction on the intermediate S-1 and substituted o-iodobenzene to obtain an intermediate S-2, and carrying out demethylation reaction on the intermediate S-2 under the action of Lewis acid to obtain S-3, 5-disubstituted benzo [B] naphthobenzene [2, 3-D] thiophene derivative. The S-3 is subjected to a ring closing reaction under the action of alkali, and the product W0: substituted benzo [B] naphthyl benzene [2, 3-D] thiophene derivative is obtained. By adopting the preparation method of the substituted benzo [B] naphthobenzene [2, 3-D] thiophene derivative provided by the invention, the obtained product is high in purity, high in yield and low in cost, no waste solvent is generated in the whole preparation process, and meanwhile, less waste water is generated, so that a foundation is laid for realizing the aim of environmental protection.

Provided herein are compositions including oxotremorine (e.g., oxotremorine methiodide or Oxo-M) and 4-PPBP (e.g., 4-PPBP maleate). Also provided are methods of treating a connective tissue defect in a subject with oxotremorine and 4-PPBP. In addition, provided are scaffolds and methods of making same that include multiple fibers that include Oxo-M, 4-PPBP, and optionally icariin or kartogenin.