16 results about "Mesitoyl chloride" patented technology

The invention discloses a tetrazine probe synthon and a preparation method and application thereof.The preparation method comprises the following steps that under the inert atmosphere, diethyl cyanomethylphosphonate, 3-hydroxypropionitrile, 3-mercaptopropionic acid and hydrazine hydrate are mixed and then react at the room temperature, a sodium nitrite solution is added after the reaction is finished, then acid is continuously added till the reaction system reaches acidity, and a tetrazine probe synthon product is obtained; continuously reacting to obtain an intermediate; and dissolving the intermediate in a solvent in an inert atmosphere, adding triethylamine, slowly adding methanesulfonyl chloride, and reacting at room temperature to obtain the tetrazine probe synthon shown in the formula I. The invention further discloses a preparation method of the tetrazine probe synthon. The tetrazine probe synthon provided by the invention can perform series Heck reaction and HWE reaction, so that controllable combination of functional groups on two sides of a tetrazine coupling probe is realized under mild reaction conditions, and the functional groups on two sides are designed according to actual requirements to regulate and control photophysical properties of the probe. A brand new way is provided for developing a high-performance biological orthogonal fluorescent probe.

The utility model belongs to the technical field of trifluoromethanesulfonyl chloride synthesis equipment, and particularly relates to multi-kettle series equipment for synthesizing trifluoromethanesulfonyl chloride, which comprises reaction kettles, a feed port and a delivery pipe, and one side of the top end of each reaction kettle is connected with the feed port. When the reaction kettle is used, three stirring vortexes are formed in the reaction kettle through the mixing mechanism, and a relative stirring mechanism is formed, so that raw materials in the reaction kettle are quickly mixed, the mixing time of the raw materials is shortened, and the working efficiency is further improved; when the raw materials are mixed, the side wall scraping rod rubs with the side wall of the reaction kettle, so that the materials adhered to the side wall of the reaction kettle can be scraped, and the materials are prevented from remaining on the side wall of the reaction kettle.

The invention relates to a preparation method of a heterocyclic compound, in particular to a preparation method of N-(5-pyrimidinemethyl)-2-pyridylamine, which comprises the following steps: (1) reacting 4, 6-dihydroxypyrimidine with N, N-dimethylformamide and phosphorus oxychloride at 20-30 DEG C for 0.5-1 hour, heating to 110-115 DEG C, and reacting for 3-4 hours to obtain 4, 6-dichloropyrimidine-5-formaldehyde; (2) reacting the 4, 6-dichloropyrimidine-5-formaldehyde with a palladium carbon catalyst and a metal salt synergistic catalyst in a hydrogen atmosphere at 40-50 DEG C for 5-6 hours to obtain 5-hydroxymethyl pyrimidine; (3) reacting the 5-hydroxymethylpyrimidine with methylsulfonyl chloride at the temperature of-5 to 5 DEG C to obtain pyrimidine-5-methyl methanesulfonate; and (4) enabling the pyrimidine-5-methyl methanesulfonate to react with 2-aminopyridine for 4 hours at the temperature of 50 to 60 DEG C, so as to obtain the N-(5-pyrimidinemethyl)-2-pyridylamine.

The invention discloses a simple synthesis method of 2, 2, 2-trifluoroethyl ether, and belongs to the field of organic synthesis. According to the synthesis method, the easily available 2, 2, 2-trifluoroethanol, trifluoromethanesulfonic anhydride / trifluoromethanesulfonyl chloride and the like are directly adopted to synthesize the 2, 2, 2-trifluoroethyl ether in one step under the action of organic alkali and under the conditions of normal temperature and normal pressure, dangerous metal / high temperature and high pressure / gas delivery is not involved, the preparation cost of the 2, 2, 2-trifluoroethyl ether is greatly reduced, and the synthesis method is suitable for an industrial production route.

This invention discloses a method for synthesizing sulfonylpyrazole, using 1-methyl-3-trifluoromethyl-5-hydroxy-1 H Using pyrazole as a raw material, under alkaline conditions, it undergoes a hydroxymethylation reaction with formaldehyde to obtain hydroxypyrazole methanol; hydroxypyrazole methanol reacts with sodium bisulfite to obtain sodium hydroxypyrazole methanesulfonate; then, under alkaline conditions, it undergoes an etherification reaction with difluorochloromethane to obtain sodium difluoromethoxypyrazole methanesulfonate; after chlorination, it obtains difluoromethoxypyrazole methanesulfonyl chloride, which then reacts with sodium sulfite to obtain sodium difluoromethoxypyrazole methyl sulfinate; finally, it undergoes a Minisci reaction with 5,5-dimethyl-4,5-dihydroisoxazole to obtain sulfonylpyrazole. This invention uses inexpensive and readily available sulfite as a sulfur source, avoiding the synthesis of 5,5-dimethyl-4,5-dihydroisoxazole sulfide compounds, reducing waste and production costs, and is easy to industrialize, thus having high practical value.

The invention discloses a method for preparing a methanesulfonate product. The method comprises the following steps: in a dichloromethane system, the reaction temperature is controlled to be no higher than 40°C and the reaction rate is controlled, a mixed solution of methanesulfonyl chloride and methanesulfonic anhydride reacts with sodium alkoxide, after the reaction is completed, the reaction solution is cooled to room temperature, filtered, dried, and subjected to rotary evaporation to remove the solvent, and distilled to obtain the methanesulfonate product. The method has a simple synthesis route, does not use an acid binding agent, a phase transfer catalyst or an esterification catalyst, does not require heating, has a short reaction time, and greatly reduces the total production cost in terms of raw materials, production cycle, environmental protection, and the like. The yield and purity of the product prepared by the method are very high, with the yield reaching above 98.2% and the purity reaching above 99.9%. The moisture content of the obtained product is also very low, and the quality of the product obtained by the method far exceeds the product standard for use as an electrolyte.

The application discloses a chlorantraniliprole reaction mother liquor recovery method and recovery processing equipment, comprising the following steps: S1: K acid and K amine are dissolved in a solvent a; S2: an acid-binding agent b is added, and temperature is controlled to drop methylsulfonyl chloride for condensation reaction; S3: after the reaction is completed, water is added to cool and crystallize; S4: centrifugation is carried out to obtain chlorantraniliprole; S5: after alkalization, the reaction mother liquor is extracted to separate an organic phase; S6: the organic phase is distilled to obtain a distillate main product; and S7: the distillate main product is dehydrated through a molecular sieve. The application has the advantages that: in the chlorantraniliprole synthesis, the selected solvent a and the acid-binding agent b can make the reaction yield greater than 94%; meanwhile, the reaction solvent a can meet the requirements of the reaction, direct separation with water, and extraction and dissolution of the acid-binding agent b in water; in the mother liquor recycling, the selected solvent a and the acid-binding agent b meet the conditions of molecular sieve dehydration, and the recovery rate of the solvent a and the acid-binding agent b is more than 95%.

The invention discloses a double-response small-molecule fluorescent probe for synchronously detecting NTR and nucleic acid and preparation and application thereof. A preparation method of the double-response small-molecule fluorescent probe comprises the following steps: adding 4-fluoro-3-methoxybenzaldehyde, potassium carbonate and methylamine hydrochloride into ethanol, and performing reflux reaction to obtain an intermediate NB1; the preparation method comprises the following steps: dissolving NB1, 4-methylpyridine and potassium tert-butoxide in N, N-dimethylformamide under the protection of nitrogen, and heating and stirring for reaction to obtain an intermediate NB2; the preparation method comprises the following steps: dissolving NB2, (4-nitrophenyl) methylsulfonyl chloride and triethylamine in dichloromethane under the protection of nitrogen, and reacting to obtain an intermediate NBP; the preparation method comprises the following steps: dissolving NBP, methyl iodide and triethylamine in dichloromethane under the protection of nitrogen, and stirring at room temperature until the reaction is completed to obtain a target product, namely the double-response small-molecule fluorescent probe. The NTR activity and the nucleic acid state in the biological sample can be synchronously and visually detected, and a more reliable technical scheme is provided for precise tumor detection and mechanism research.

This invention relates to a method for preparing a heterocyclic compound, specifically to a method for preparing N-(5-pyrimidinylmethyl)-2-pyridineamine, comprising the following steps: (1) reacting 4,6-dihydroxypyrimidine with N,N-dimethylformamide and phosphorus oxychloride at 20-30°C for 0.5-1 hour, and then heating to 110-115°C for 3-4 hours to obtain 4,6-dichloropyrimidin-5-carboxaldehyde; (2) reacting 4,6-dichloropyrimidin-5-carboxaldehyde with palladium on carbon catalyst and metal salt co-catalyst in a hydrogen atmosphere at 40-50°C for 5-6 hours to obtain 5-hydroxymethylpyrimidine; (3) reacting 5-hydroxymethylpyrimidine with methanesulfonyl chloride at -5-5°C to obtain methyl pyrimidin-5-methanesulfonate; (4) reacting methyl pyrimidin-5-methanesulfonate with 2-aminopyridine at 50-60°C for 4 hours to obtain N-(5-pyrimidinylmethyl)-2-pyridineamine.

The utility model belongs to the technical field of trifluoromethanesulfonyl chloride synthesis equipment, and particularly relates to fixed bed equipment for synthesizing trifluoromethanesulfonyl chloride, which comprises a fixed bed reactor and a feed pipe, one side of the fixed bed reactor is sequentially connected with the feed pipe and an air inlet pipe, and the inner side of the fixed bed reactor is sequentially provided with a cyclone separator, a heat exchange pipe and a reaction bed. One end of the feeding pipe is movably connected with the distributor through a bearing, the distributor is movably connected with the first support through a bearing, the first support is fixed to the inner side of the fixed bed reactor, a connecting rod is fixed to the lower side of the distributor, and a second support and a third support are sequentially fixed to the side, close to the lower end of the connecting rod, of the fixed bed reactor. With the adoption of the device, the synthesis efficiency of trifluoromethanesulfonyl chloride can be improved.

This invention discloses a synthesis process and equipment for chlorantraniliprole, comprising the following steps: S1: mixing ketalic acid, ketamine, and solvent, adding an acid-binding agent, stirring until dispersed and mixed, and then adding methanesulfonyl chloride dropwise to react and obtain a mixture containing chlorantraniliprole; S2: adding water to the mixture containing chlorantraniliprole, stirring, centrifuging, and rinsing with water to obtain crude chlorantraniliprole; S3: adjusting the alkali and removing the solvent from the centrifuged mother liquor in S2 to obtain a usable acid-binding agent and solvent; S4: rinsing the crude chlorantraniliprole with methanol and drying to obtain the chlorantraniliprole. This invention simplifies the recovery reaction steps of the acid-binding agent and solvent by separating the centrifuged mother liquor and crude chlorantraniliprole through centrifugation and rinsing with water, and then adjusting the alkali and removing the solvent from the centrifuged mother liquor to obtain a usable acid-binding agent and solvent, saving time and effort, and is simple to operate.

The invention provides a method for preparing benzovindiflupyr, which comprises the following steps of: in the presence of alkali and a solvent, mixing 3-difluoromethyl-1-methyl-1H-pyrazole-4-carboxylic acid and 9-dichloromethylene-1, 2, 3, 4-tetrahydro-1, 4-bridge methylene-naphthalene-5-amino together to form a material I, dropwise adding methylsulfonyl chloride into the material I, and reacting at the temperature of between 20 and 30 DEG C to obtain the benzovindiflupyr. After the reaction, the reaction product is directly filtered and dried to obtain the benzovindiflupyr, the method is simple, efficient and environment-friendly, and the benzovindiflupyr with high purity and high yield is provided.

The application discloses a synthesis method of 2-furanpropionic acid ethyl ester, and belongs to the technical field of synthesis of spices and pharmaceutical intermediates. Furfuryl alcohol and methylsulfonyl chloride are reacted to obtain a methyl sulfonate intermediate, then the methyl sulfonate intermediate is subjected to a bromination reaction to obtain 2-bromomethyl furan; under the action of a strong base, the 2-bromomethyl furan is reacted with ethyl acetate to obtain a product 2-furanpropionic acid ethyl ester. The synthesis method of 2-furanpropionic acid ethyl ester provided by the application is economical in reagents, mild in reaction conditions, safe in reaction process, high in reaction yield (up to 94%) and high in product purity (up to 99%), and is suitable for industrial production.

The invention belongs to the technical field of pharmaceutical chemicals, and particularly relates to chiral R-styralyl acetate and a preparation method thereof. The chiral R-styralyl acetate is subjected to functional modification through methylsulfonyl chloride, high-selectivity inhibition on COX-2 is realized through dihydrogen bond anchoring, the inhibition rate of a non-steroidal drug on COX-1 is reduced, and adverse reaction on gastrointestinal tracts after the non-steroidal drug is taken for a long time is relieved; a free radical bromination system composed of N-bromo-succinimide and benzylamine peroxide is adopted to replace traditional bromine, meanwhile, a triphenylphosphine ligand is introduced to serve as a steric hindrance modifier, a dynamic space barrier is constructed near alpha-C by reducing specific bromination activation energy at the alpha position, a halogen free radical attack path is limited in the alpha-C direction, and the steric hindrance modification effect is achieved. The conversion rate of the chiral R-styralyl acetate is increased, so that the obtained chiral R-styralyl acetate non-steroidal drug has both high drug effect and low gastrointestinal toxicity.

The invention discloses a synthesis process of N-(5-methoxy-2-phenoxy phenyl) methanesulfonamide, which takes 1-chloro-4-methoxy-2-nitrobenzene as an initial raw material, and comprises the following steps: (1) nucleophilic aromatic substitution reaction: in the presence of alkali and a solvent, carrying out a reaction for 2-4 hours to obtain 2-(5-methoxy-2-phenoxy phenyl) methanesulfonamide; the preparation method comprises the following steps: reacting 1-chloro-4-methoxy-2-nitrobenzene with phenol to generate 4-methoxy-2-nitro-1-phenoxybenzene; (2) nitro reduction reaction: in the presence of a catalyst and hydrogen, reducing the 4-methoxy-2-nitro-1-phenoxybenzene into 5-methoxy-2-phenoxyaniline; and (3) a methylsulfonylation reaction: in the presence of alkali and a solvent, enabling the 5-methoxy-2-phenoxyaniline to react with methylsulfonyl chloride to generate the N-(5-methoxy-2-phenoxyphenyl) methanesulfonamide. The product provided by the invention has the advantages of high purity and high yield, and can meet the requirements of industrial production on product quality and yield.

The invention provides a preparation process and a decoloration purification method of p-hydroxybiphenyl nitrile for display, and belongs to the technical field of organic synthesis and preparation of liquid crystal material intermediates. Aiming at the defects of high cost, low yield and poor product purity of the existing process, the invention adopts the innovative design of three-step core reaction and four-step decoloration purification: methylsulfonyl chloride is used for replacing benzene sulfonyl chloride to realize hydroxyl low-cost protection, and the isomer content 1t is controlled through four-section gradient heating bromination reaction; and decoloring and purifying by a four-step method of ethanol extraction, activated carbon decoloring, EDTA (Ethylene Diamine Tetraacetic Acid) complexing, alumina column chromatography and DMF (Dimethyl Formamide) / dichloroethane recrystallization. The method has the beneficial effects that the raw material cost is obviously reduced compared with that of a traditional process, and the total molar yield is increased from 48% to 60%; the product purity reaches 99.8%, the chromaticity L value is 92, and the heavy metal residue is 1t; the method overcomes the defects of high cost, low yield, difficulty in decolorization and the like of the traditional process, and the used raw materials and equipment are chemical conventional categories, have definite steps and can be industrially amplified.