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739 results about "Dimethyl sulfate" patented technology
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Dimethyl sulfate is a chemical compound with formula (CH₃O)₂SO₂. As the diester of methanol and sulfuric acid, its formula is often written as (CH₃)₂SO₄ or even Me₂SO₄, where CH₃ or Me is methyl. Me₂SO₄ is mainly used as a methylating agent in organic synthesis.
Cationic asphalt emulsifier and preparation method and application thereof
ActiveCN101745340AWide selectionWide applicabilityTransportation and packagingMixingChloroacetic acidsFatty alcohol
The invention relates to cationic asphalt emulsifier and preparation method and application thereof. The main agent of the cationic asphalt emulsifier is prepared through the reaction of quaternarization reagent and intermediate at molar ratio of 0.5-3:1, wherein the intermediate is produced in the reaction of organic acid mixture and organic amine at molar ratio of 1: 1-3. The adjuvant agent of the cationic asphalt emulsifier is the combination of, based on the main agent by weight, 0.1-2.5% of nonionic surfactant and 0.1-2.5% of modifier. The organic acid mixture is the mixture of linear, branched or naphthene-containing organic acid with small relative pace steric effect and organic acid with big relative space steric effect at molar ratio of 1: 3- 3: 1. The quaternarization reagent is epichlorohydrin, hydrochloric acid, chloromethane, dimethyl sulfate or chloroacetic acid. The modifier is one or more of aluminum sulfate, ammonium chloride and calcium chloride and the nonionic surfactant is fatty alcohol-polyoxyethylene ether. The emulsifier has no bad effects to the property of the asphalt, has wide application range and can satisfy different construction conditions.
Owner:PETROCHINA CO LTD +1
Preparation method of Ibrutinib
ActiveCN103626774AEase of industrial productionRaw materials are easy to getOrganic chemistryCyanideBenzoyl chloride
The invention discloses a preparation method of Ibrutinib (I). The preparation method comprises the following steps: performing condensation and methyl oxidization reaction on 4-phenoxyl benzoyl chloride (II) serving as a raw material and methylene cyanide and dimethyl sulfate to generate 4-phenoxyl phenyl (methoxyl) ethenylidene dicyan methane (III); performing pyrazol cyclization reaction between the intermediate (III) and 1-(3R-diazanyl-1-piperidyl)-2-propylene-1-ketone(IV) to obtain 1-[(3R)-[3-(4-phenoxyl phenyl)-4-nitrile-5-amino-1H-pyrazolyl]-1-piperidyl]-2-propylene-1-ketone(V). The pyrimidine cyclization reaction between the intermediate (V) and a cyclization agent is performed to prepare the Ibrutinib (I). The preparation method has easily-available raw materials, and is simple in process, economical and environment-friendly, and suitable for industrial production.
Owner:TONGLING WANGYANTANG BIOTECHNOLOGY CO LTD
Methylsulfonic acid preparing process
InactiveCN1810780ANo pollution in the processRaw materials are easy to getSulfonic acid preparationSulfate radicalsWater insoluble
The environment friendly methyl sulfonic acid preparing process includes the following steps: the reaction of the water solution or solid of ammonium sulfite or mixture of ammonium sulfite and ammonium bisulfite with dimethyl sulfate at high temperature to produce ammonium methyl sulfonate; treating the reacted solution containing ammonium methyl sulfonate and ammonium sulfate with calcium hydroxide or other compound capable of producing precipitate with sulfate radical ion to produce water soluble calcium methyl sulfonate, water insoluble calcium sulfate and ammonium hydroxide; treating obtained calcium methyl sulfonate with strong acid capable of forming precipitate with calcium ion; and final decompression distilling to obtain methyl sulfonic acid. The present invention has facile material, simple technological process, high product quality, low cost and no environmental pollution, and is suitable for industrial production.
Owner:HEBEI YANUO CHEM IND
Clean carbon dioxide foam fracturing fluid and preparation method thereof
ActiveCN104531129AFine foamImprove foam stabilityDrilling compositionPotassium persulfatePolymer science
The invention discloses clean carbon dioxide foam fracturing fluid and a preparation method thereof, and relates to the technical field of oilfield chemistry and fracturing production increase. The carbon dioxide foam fracturing fluid is mainly composed of a base solution, a foaming agent, a gel breaker and liquid carbon dioxide with the mass ratio being 100 to 0.15-0.45 to 0.02-0.08 to 100-900. The base solution is formed by 0.2%-0.55% of a thickening agent and water. The thickening agent is mainly formed by bisacrylamide, vinyl pyrrolidone, kation unsaturated monomer, anion unsaturated monomer, an initiator, sodium carbonate, an emulsifying agent and a hydrotropy agent. The foaming agent is mainly formed by hexadecyl dimethyl tertiary amine, dimethyl sulfate, caustic soda flakes, potassium persulfate and solvent. The clean carbon dioxide foam fracturing fluid has the advantages of being high in foam stability, high in temperature resistance and shear resistance, high in sand-carrying performance, wide in applicable temperature range, extremely low in residue content, high in backflow performance, and small in secondary damage to a reservoir after fracturing, thereby improving the fracturing effect and increasing the reservoir productivity.
Owner:CHENGDU BAICHUN PETROLEUM TECH
Synthesis of fluorescence enhanced fluorescent molecular probe for detecting mercapto-containing amino acids, and application of probe
InactiveCN103351335AHigh sensitivityGood optical performanceOrganic chemistryMaterial analysis by observing effect on chemical indicatorAA - Amino acidFluorescence spectrometry
Owner:CENT SOUTH UNIV
Preparation method of taxanes compound
ActiveCN102060815AShort preparation timeImprove reaction efficiencyOrganic chemistryDocetaxelCabazitaxel
The invention discloses a preparation method of a taxanes compound shown as the formula I in the specification, relating to the field of pharmaceutical chemistry. The preparation method comprises the following steps of: under the water isolating condition, with docetaxel as a raw material and benzene alcohol, ketons or ethers compounds as a solvent, dropwise adding dimethyl sulfate, carrying out the alkylation reaction for 0.5 to 10 hours at the temperature of 10 to 60 DEG C, controlling the PH value of the reaction solution between 7 and 8 by an alkalescent organic solvent during the alkylation reaction, and adding water for separate out crystals after the alkylation reaction, wherein the crystals are the compound shown as the formula I. In the preparation method, a one-step method is adopted to prepare the taxanes compound cabazitaxel shown as the formula I. The preparation method has the advantages of few reaction steps, mild reaction condition, short reaction time and high reaction efficiency, and is favorable for industrial production. Meanwhile, through controlling the dropping speed of an alkylating agent and the PH value of the reaction solution, the docetaxel can be prevented from decomposing and the purity of the reaction product can be enhanced.
Owner:重庆兴泰濠制药有限公司
Quaternary ammonium salt in ester-amines and synthetic method
InactiveCN1562960ARaise the gradePromote degradationOrganic compound preparationAmino-hyroxy compound preparationQuaternary ammonium cationMethyl carbonate
In this invention, fatly acid and ethanolamine are proportioned and under ester-aminated, then reacting with dimethyl carbonate to produce ester-amine type quaternary ammonium salt. Said invention p rocess of synthesis has high transforming rate, excellent selectivity, high content of active matter in said product, utilizing no pollution type raw material of dimethyl carbonate, so, no remaining of poison in product, lowering quaternary ammonium salt pollution to environment and to human health.
Owner:CHINA RES INST OF DAILY CHEM IND
Polymeric chelant and coagulant to treat metal-containing wastewater
The present invention is directed to the use of a combination of a polymeric chelant and coagulant to treat metal containing wastewater. More particularly, the invention is directed at removing copper from CMP wastewater. The composition includes a combination of (a) a polymeric chelant derived from a polyamine selected from the group consisting of diethylenetriamine (DETA), triethylenetetraamine (TETA), tertraethylenepentaamine (TEPA), poly[vinylamine], and branched or linear poly[ethylenimine] (PEI); and (b) a water soluble or dispersible copolymer of a tannin and a cationic monomer selected from the group consisting of methyl chloride or dimethyl sulfate quaternary salt of dimethyl aminoethyl acrylate, diethylaminoethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, dimethylaminopropyl methacrylamide, dimethylaminopropyl acrylamide, and diallyl dimethyl ammonium chloride.
Owner:GENERAL ELECTRIC CO
Pyraclostrobin and method for economically synthesizing same
InactiveCN102399190AIncrease profitReduce energy consumptionBiocideOrganic chemistryCarbamateSolvent
The invention aims to provide pyraclostrobin and a method for economically synthesizing the same. High purity pyraclostrobin can be synthesized at low cost. The method comprises the following steps of: adding N-hydroxy-N-2-[(N-parachlorobenzyl)-3-pyrazoloxymethyl]phenyl carbamate and an acid bonding agent into a polar solvent or non-polar solvent, uniformly mixing, adding dimethyl sulfate, and reacting at the temperature of between 20 and 30DEG C; and after the reaction is monitored to be finished through high performance liquid chromatography (HPLC), adding water to neutralize until the pH=7, removing the solvent, immersing in a recrystallization solvent, performing recrystallization, and removing a recrystallization solution to obtain the pyraclostrobin, wherein a molar ratio of the N-hydroxy-N-2-[(N-parachlorobenzyl)-3-pyrazoloxymethyl]phenyl carbamate to the acid bonding agent to the dimethyl sulfate is 1:(1-1.8):(1-1.8). By the invention, the energy consumption is low, the utilization rate of materials is high, the operation is simple, and the yield and purity of the product are high; and compared with the traditional method, the method is more energy-saving, environment-friendly and economic, and has great industrial application value.
Owner:HENAN UNIV OF CHINESE MEDICINE
Ore dressing collector and preparation method thereof
The invention discloses an ore dressing collector and a preparation method thereof. The ore dressing collector consists of the following raw materials in percentage by weight: 75 to 80 percent of oleic acid, 3 to 5 percent of surfactant, 5 to 7 percent of N,N-dimethylformamide-dimethyl sulfate, and 10 to 15 percent of chloride. The oleic acid is subjected to electrolytic dissociation and chemicalmodification by the steps of activation, electrolyzation, separation and introduction of an active group so as to form the ore dressing collector with high activity, dispersibility and selectivity. The ore dressing collector is particularly suitable for ore dressing of minerals such as non-metallic fluorite, kyanite, barite, metal white tungsten, hematite reverse flotation and the like, particularly the ore dressing at low temperature (more than or equal to 2 DEG C).
Owner:烟台市富林矿山机械有限公司
Chitooligosaccharide quaternary ammonium salt and its synthesis method
InactiveCN102690297ALow priceHigh degree of quaternizationBiocideSugar derivativesSynthesis methodsStructural formula
The invention provides a chitooligosaccharide quaternary ammonium salt with a structural formula as formula (1). The preparation method of the chitooligosaccharide quaternary ammonium salt comprises the following steps of: taking a mixture of dimethyl sulfate and water as a solvent and dimethyl sulfate as a methylation reagent; during preparation, adding chitooligosaccharide into the solvent to prepare a chitooligosaccharide solution, then adding NaOH and NaCl into the solution, and conducting magnetic stirring for reaction at room temperature; precipitating the reaction solution with acetone, carrying out pumping filtration, filter cake washing, and drying, thus obtaining the chitooligosaccharide quaternary ammonium salt. The chitooligosaccharide quaternary ammonium salt of the invention has the quaternary ammonium group grafted to the chitooligosaccharide, and has strengthened bacteriostatic activity as well as its own advantages, thus boasting broad application prospects. The method of the invention adopts dimethyl sulfate as the methylation reagent which is characterized by inexpensiveness and low toxicity, and has the advantages of mild reaction condition, no need for other reaction solvent, high reaction efficiency, and simple reaction process, thus being conducive to mass production.
Owner:连云港海康生物科技有限公司
Method for realizing selective N-methylation of primary amine
InactiveCN103172523ANo harmImprove economyOrganic compound preparationSulfonic acid amide preparationIridiumNitrogen gas
The invention relates to a method for realizing selective N-methylation of primary amine, which comprises the following steps: in a nitrogen gas protective atmosphere or in the air, adding a primary amine derivative, a metal iridium or ruthenium complex, methanol and alkali into a reaction vessel; reacting the reaction mixture at 100-150 DEG C for several hours, and then cooling to room temperature; and performing rotary evaporation to remove the solvent, and then performing column separation to obtain a target compound. Compared with the prior art, the reaction shows the following remarkable advantages: 1) the methanol is used as an alkylation agent, thereby avoiding the use of virulent haloalkane and dimethyl sulfate; 2) the reaction only generates water as the byproduct, thereby causing no environmental hazard; 3) the reaction is high in atom economy; 4) the reaction shows absolute selectivity, and the reaction only generates mono-methyl products and generates no bis-methyl products; and 5) the reaction shows wide substrate universality and is effective for various primary amine derivatives.
Owner:NANJING UNIV OF SCI & TECH
Cyanoacrylate derivatives and their preparation method and biological activity
This invention discloses a medicine of anti-tumor and anti-plant virus effect---- cyanoacrylate category derivative and its preparing method and biological activity. The following general formula denotes the compound and its preparing method. The definition of R1, R2, R3 in the formula is in instruction book. Materials are carbon bisulfide, cyan acetic ester, dimethyl sulfate, aromatic amine, and sodium cyanide is catalyst, cyanoacrylate category derivative is synthesized by three steps. There is proliferation inhibitory effect of compound b, k to PC3 prostate cancer cell gene stock, and proliferation inhibitory effect of compound i, j to NIN3T3 cell ERK albumen phosphorylation, and good anti-cancer activity is revealed. There is inhibitory activity of compound b, n to tobacco mosaic, and certain anti-plant virus activity is revealed.
Owner:GUIZHOU UNIV
Synthetizing method of lacosamide
InactiveCN103113256AHighlight substantive featuresSignificant progressOrganic compound preparationCarboxylic acid amides preparationPtru catalystAmmonium chloride mixture
The invention provides a synthetizing method of lacosamide. The method comprises the steps of: based on D-serine as a raw material, performing an acylation reaction with acetic anhydride and then performing a condensation reaction with benzylamine; and finally, performing a methylation reaction with dimethyl sulfate, thereby obtaining lacosamide, wherein N,N' dicyclohexylcarbodiimide (DCC) or N,N' carbonyl diimidazole (CDI) is used as a catalyst in the condensation reaction; and a phase transfer catalyst including triethyl benzyl ammonium chloride (TEBA), tetrabutylammonium chloride (TBAC), tetrabutylammonium bromide (TBAB) or tetrabutylammonium hydrogen sulfate (TBAHS) is adopted in the methylation reaction. The method has the advantages of being simple in synthetizing process, moderate in reaction condition, simple in after-treatment, high in yield and high in product purity.
Owner:SUZHOU HONGRUI MEDICAL TECH
Method for synthesizing methoxamine hydrochloride
ActiveCN101357895AReduce usageImprove the operating environmentOrganic chemistryHalohydrocarbonHydroxylamine Hydrochloride
The invention provides a method for synthesizing methoxyamine hydrochloride and includes the following steps: ethyl acetate and hydroxylamine hydrochloride are added into a reaction vessel and 10 to 30 percent of sodium hydroxide solution is instilled for oximation reaction; then dimethyl sulfate is instilled, and at the same time sodium hydroxide solution with the mass fractions of 10 to 30 percent is instilled for methylation reaction; cold water is added after the temperature is decreased and a halohydrocarbon solvent is adopted for extraction; pressure is reduced under the temperature of 30 to 50 DEG C to recover the halohydrocarbon solvent and the product obtained is added into inorganic acid solution for hydrolysis reaction; after the hydrolysis is over, hydrochloride is used to obtain the product methoxyamine hydrochloride. The synthetic method which is simple improves the operation environment and increases the yield ratio.
Owner:JIANGSU QINGQUAN CHEM CO LTD
Imidazoline quaternary ammonium salt corrosion inhibitor and preparation method thereof
InactiveCN109053579ALow toxicityImprove release efficiencyOrganic chemistryBenzoic acidDiethylenetriamine
The invention discloses an imidazoline quaternary ammonium salt corrosion inhibitor which is prepared from the following preparation raw materials including a corrosion inhibitor main component raw material and an additive raw material; the corrosion inhibitor main component raw material is one of oleic acid, benzoic acid, fatty acid, lauric acid and natural eleostearic acid; and the additive rawmaterial includes diethylenetriamine, dimethyl sulfate or benzyl chloride, boric acid and xylene. The invention also discloses a preparation method of the imidazoline quaternary ammonium salt corrosion inhibitor and aims at solving the problem of poor corrosion inhibition performance of the existing corrosion inhibitor in an acid medium. The preparation method is simple, is liable to operate and can perform recovery utilization on a solvent. An imidazoline corrosion inhibitor has the advantages of low toxicity, high slow release efficiency and wide use range. Physical characterization and performance test results of the corrosion inhibitor show that oleic acid imidazoline quaternary ammonium salt has better slow release performance, and the slow release performance of the benzyl chloride is better than the slow release performance of the dimethyl sulfate after being quaternized. A polarization curve test shows that synthesized corrosion inhibitors are all cathodal depression type corrosion inhibitors.
Owner:YANAN UNIV
Process for producing methanesulfonic acid
ActiveCN101219975AEfficient use ofEasy to produceSulfuric acid esters preparationAlkaline earth metalEvaporation
The invention discloses a preparation method for methanesulfonic acid. A water liquor or a solid mixture of a sulfite or a mixture of the sulfite and a bisulfite is reacted with a dimethyl sulfate to generate a methylsulfonate and a sulfate, and the mixture liquor of the reaction directly cools and precipitates a sulfate salt crystallization through concentration by adding a salting-out agent or a concentrated liquor; filtering and removing a dilute-methyl sulfonate liquor of the sulfate; a soluble alkaline earth salt can also be reused as a precipitant for further removing the remained sulfate ion; finally, the purified methylsulfonate liquor is concentrated to pulpiness or dry powder to be acidified by excess concentrated hydrochloric acid or excess hydrogen chloride gas is directly pumped in the purified methylsulfonate liquor to precipitate a sodium chloride crystallization. After filtering, the mixed acid liquor of hydrochloride and methanesulfonic acid can be gotten, which can get the highly-purified methanesulfonic acid after evaporation concentration, vacuum distillation and distillation. The materials of the invention can be gotten easily and the invention has simple techniques and low cost, which does no harm to the environment and is suitable to be used in industry.
Owner:HEBEI YANUO CHEM IND
Fibriuretinin synthesis method
ActiveCN102040604AOptimizationSimple purification methodOrganic chemistryChemical synthesisBerberine
The invention relates to a fibriuretinin synthesis method. The method takes berberine hydrochloride as a starting material and comprises the following steps: selectively carrying out decomposition reaction on methylenedioxy of the berberine hydrochloride to obtain ortho-dyhydroxyl berberine hydrochloride; carrying out methylation reaction on hydroxyl of the ortho-dyhydroxyl berberine hydrochloride and dimethyl sulfate, recrystallizing, and adding hydrochloric acid to regulate pH value to obtain the target product, i.e. fibriuretinin. The fibriuretinin synthesis method has less synthesis steps, simple technology, and high total yield of 49.3% and the raw materials are easy to collect, so as to reduce cost, improve production efficiency and contribute a new synthesis method for fibriuretinin chemosynthesis industrialization.
Owner:YUNNAN PHYTOPHARML
Method for preparing loxoprofen intermediate
InactiveCN105753685AAvoid bringing inHigh selectivityCarboxylic acid nitrile preparationOrganic compound preparationPropanoic acidPropionitrile
A method for preparing a loxoprofen intermediate comprises the following steps that 1, on the presence of sodium alkoxide, benzyl cyanide and dimethyl carbonate are subjected to methylation in an organic solvent, and 2-(phenyl cyano) sodium propionate is obtained; 2, 2-(phenyl cyano) sodium propionate and dimethyl sulfate react in an organic solvent to obtain 2-(phenyl cyano) methyl propionate; 4, 2-(phenyl cyano) methyl propionate reacts under the alkaline condition to obtain 2-phenyl propionitrile; 4, 2-phenyl propionitrile is hydrolyzed under the alkaline condition, acid is added for acidizing after the reaction to obtain 2-phenylpropionic acid; 5, 2-phenylpropionic acid, hydrobromic acid and paraformaldehyde are mixed and subjected to a bromine methylation reaction under the acidic condition, and 2-(4-tribromomethyl phenyl) propionic acid is obtained.According to the method, a new synthesis route is designed, product selectivity is good, the purity is high, the conversion rate is high, and few by-products are generated; the raw materials are simple and easy to obtain, the production conditions are mild, the process is simple, production cost is low, and pollution is small.
Owner:UPCHEM CHINA
Production process of methyl p-tolyl sulfone
InactiveCN101434566AReduce the risk of contaminationReduce manufacturing costOrganic chemistryOrganic compound preparationChlorideToluene
The invention relates to a manufacturing technology of pharmaceutical intermediates, in particular to a manufacturing technology of P-methylsulfonyl toluene. The invention provides a manufacturing technology of the P-methylsulfonyl toluene, which includes the following steps: (1) the salt-forming reaction of P-methylsulfonyl sulfonic acid chloride; and (2) the methylation reaction of P- toluene sodium sulfinate generated in step (1), wherein step (2) is that P-methylsulfonyl sulfonic acid chloride reacts with monochloro methane to generate the P-methylsulfonyl toluene which is shown as a reaction formula (c). Compared with the conventional technology, the technology has two very distinct advantages: firstly, a two-step reaction method replaces the conventional three-step reaction method so as to greatly reduce the production costs and cycle; and secondly, monochloro methane with low toxicity replaces explosive dimethyl sulfate with high toxicity, thereby not only reducing the risk of environmental pollution and being more in line with the requirements of environmental protection, but also greatly improving labor conditions and being more conducive to safe production.
Owner:ANJI HAOSEN PHARMA
Method for synthesizing imidazoline intermediate and cationic derivative thereof
The invention relates to a method for synthesizing an imidazoline intermediate and a cationic derivative thereof. The method comprises the following process steps of: putting fatty acid, polyamine and water into a reaction kettle in a mole ratio of 1:1.1-2:1-5, heating to the temperature of between 100 and 180 DEG C to distill over the water added before and the water generated in the reaction, removing redundant polyamine and water under a pressure of between -0.04 and -0.1MPa and performing a reaction at a temperature of between 180 and 240 DEG C for 3 to 8 hours to synthesize the imidazoline intermediate; and reducing the temperature of the imidazoline intermediate to be below 80 DEG C, adding a solvent of which the mass is 30 to 100 percent of the imidazoline intermediate into the imidazoline intermediate, then adding 1 to 2mol of sulfate into the mixture and performing heat preservation reaction at the temperature of between 50 and 80 DEG C for 2 to 4 hours to synthesize cationic imidazoline. The fatty acid is oleic acid, linoleic acid, stearic acid, palmitic acid, lauric acid, coconut oil acid, capric acid and octanoic acid; the polyamine is ethylenediamine, diethylenetriamine, triethylene tetramine and tetraethylene pentamine; the solvent is isopropanol, absolute ethyl alcohol or 95 percent ethanol; and the sulfate is dithyl sulfate and dimethyl sulfate.
Owner:苗俊良
Para-(2-methoxyl) ethylphenol synthesis method
ActiveCN1800128AThe reaction route is simpleThree wastes lessEther preparation from oxiranesTyrosolMethyl carbonate
The invention discloses a method for synthesizing phenetyl, which uses p-chlorophehol or p-bromophenol as starting reaction raw material. It first uses methyl, benzyl or tert-butyl to protect the phenolic hydroxyl, the parivis which is protected by the phenolic hydroxyl reacts with the magnesium in the ether, tetrahydrofuran, tert-butyl methyl ether, isopropyl ether and its mixing solution to obtain the Grignard reagent, the Grignard reagent directly reacted with the etox to obtain the tyrosol which is protected by the phenolic hydroxyl, the tyrosol reacts with the dimethyl sulfate, dimethyl carbonate, trimethyl orthoformate to obtain the tyrosol ether which is protected by phenolic hydroxyl, which obtains the product in acid or hydrogenation protection.
Owner:SHANDONG HANXING PHARM TECH CO LTD +1
Process for preparation of amisulpride
The present invention is related to a novel process for the preparation of amisulpride (I) which involves: methylation of 4-amino-salicylic-acid (VI) with dimethyl sulphate and base, optionally in presence of TBAB to obtain 4-amino-2-methoxy methyl benzoate (VII) and (ii) oxidation of 4-amino-2-methoxy-5-ethyl thio benzoic acid (IX) or 4-amino-2-methoxy-5-ethyl thio methyl benzoate (X) with oxidizing agent in the presence of sodium tungstate or ammonium molybdate to give 2-methoxy-4-amino-5-ethyl-sulfonyl benzoic acid (IV) or 2-methoxy-4-amino-5-ethyl-sulfonyl methyl benzoate (XI) respectively.
Owner:LUPIN LTD
Synthetic process of hexazinone
ActiveCN103755654AOmit extractionReduce extractionOrganic chemistrySodium methoxideChemical reaction
The invention provides a synthetic process of hexazinone. The synthetic process comprises the steps of: by taking ethanol, lime nitrogen, cyclohexylamine, dimethylamine, dimethyl sulfate, sodium methoxide and phosgene as main active ingredients, generating a series of chemical reactions in solvent, and carrying out desolventizing and concentration, crystallizing and separating and drying to obtain a finished hexazinone product. According to the synthetic process, the solvent extraction can be omitted, the reaction procedures can be reduced, the efficiency can be improved, the energy consumption can be saved by 10%, and the conversion rate can also be improved by 5%; while the amount of waste water can be greatly decreased, dimethylamine can be recycled, and the quality of solvent can be guaranteed; a great amount of water can be saved, therefore, the production cost can be greatly lowered.
Owner:ANHUI GUANGXIN AGROCHEM
Method of producing toltrazuril
A preparation method of the Toltrazuril is provided. The Toltrazuril is the 1-[3-methyl-4-(4- Trifluoromethylthiobenzoxy) benzyl]-3-methyl-1, 3, 5, -triazine-2, 4, 6(1H, 3H, 5H)-trione. The methyl sulfide chloro compounds, fluoro-compounds, amides, phenol, methyl nitrate chlorobenzene, benzene aether, ammonia benzene aether, isonitrile acid ester and methyl urea from the reactions of 4-nitrochlorobenzene, sulfur, sodium sulfide and dimethyl sulfate. The detailed preparation is that reaction 1: the methanol of 410g and 4-nitrochlorobenzene of 158g are mixed and heated until soluble and are added with sulfur, sodium sulfide and methanol mixed liquor by drops, and kept for 2h under temperature of 60 DEG C. to 65DEG C.; reduce the temperature, add water of 880g and add dimethyl sulfate of 192g; during the period, the pH value of the sodium hydroxide is adjusted over 9, and the methyl sulfide of 153.6 is gained by filtering after reaction with yield of 91.1 per cent.
Owner:PU LIKE BIO ENG +1
Synthesis method of taxane drug 7, 10-methoxy-docetaxel
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.
Owner:无锡紫杉药业股份有限公司
Preparation method of methyl p-tolyl sulfone
InactiveCN101659635AHighlight substantiveSignificant progressOrganic chemistryOrganic compound preparationSodium bicarbonateMethylating Agent
The invention relates to a preparation method of methyl p-tolyl sulfone, which belongs to the technical field of sulphone preparation, in particular to a preparation method of the methyl p-tolyl sulfone by taking monochloro methane as a methylating agent for synthesis. The preparation method is characterized by taking p-toluenesulfonylchloride, anhydrous sodium sulfite, sodium bicarbonate and monochloro methane as synthesizing raw materials and comprising the following operation steps: a. salifying the p-toluenesulfonylchloride; b. synthesizing the methyl p-tolyl sulfone; c. adjusting pH, reducing the temperature and discharging; d. filtering, dehydrating and drying; and e. inspecting the quality and packaging and warehousing after qualification. The invention provides a preparation methodof the methyl p-tolyl sulfone without using a deadly poisonous compound of dimethyl sulfate as a raw material, and has safe operation, environmental protection, short production period, good productquality, high yield, low production cost and strong market competitiveness. The content of the methyl p-tolyl sulfone reaches up to 99.5 percent, and the yield of the methyl p-tolyl sulfone, which iscounted by the p-toluenesulfonylchloride of the raw material, is more than or equal to 85 percent.
Owner:SHANDONG XINGHUI CHEM
Method for preparing o-methoxybenzaldehyde by use of micro-reaction device
ActiveCN104447246ALarge specific surface areaIncrease transfer rateOrganic compound preparationCarbonyl compound preparationMicroreactorOrganic solvent
The invention discloses a method for preparing o-methoxybenzaldehyde by use of a micro-reaction device. The method comprises the following steps: dissolving salicylaldehyde into the aqueous solution of a strong base to obtain a homogeneous solution; dissolving dimethyl sulfate into an organic solvent to obtain a homogeneous solution; simultaneously pumping the two homogeneous solutions into the micro-reaction device, respectively, and reacting at a temperature within the range of 70-120 DEG C for 1-10 minutes; and collecting the liquid effluent, namely the crude product of o-methoxybenzaldehyde. The micro-reaction device has the characteristics of large specific surface area, high transfer rate, short contact time, low by-product, excellent heat transfer and mass transfer capacity, fast and direct amplification, high safety, good operability and the like.
Owner:NANJING UNIV OF TECH
Synthetic method for propylend glycol dimethyl ether
InactiveCN1554632AHigh selectivityMild reaction conditionsEther preparationMethyl carbonatePotassium hydroxide
The synthesis process of propylene glycol dimethyl ether features that the materials including propylene glycol methyl ether, alkali and alkylation agent are reacted at 40-90 deg.c to prepare propylene glycol dimethyl ether product. Where, the alkali may be sodium hydroxide, sodium methoxide, potassium hydroxide or potassium methoxide; and the alkylation agent may be chloromethane, dimethyl sulfate or dimethyl carbonate. The present invention has the advantages of mild reaction condition, high production safety, high product selectivity, less side reactions, high product purity, simple technological process, and easy industrial application.
Owner:NANJING FORESTRY UNIV +1
Method for synthesizing nusaturated hydrophilic methyl or ethyl end capping polyether
In the synthetic method, allyl alcohol polyether and dimethyl sulfate or diethyl sulfate are etherified at temperature of 0-80 deg.C, under action of basic microcapsule catalyst in slow release and unsaturated hydrophilicity methyl or ethyl end capped polyether is obtained after neutralizing with acid-base and washing. The catalyst slowly releases alkali microcapsule prepard by alkali metal hydroxide or by mixed alkali metal chamicals.
Owner:王伟松
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