21 results about "Chlorethoxyfos" patented technology

The invention relates to the field of cables, and discloses an aerial insulated cable, a protective layer of which is prepared from the following materials: low-density polyethylene, nitrile rubber, ethylene-vinyl acetate copolymer, modified composite filler, functional additive and the like. The modified composite filler is prepared by grafting a modified silane coupling agent and Na-montmorillonite loaded titanium dioxide; the modified silane coupling agent is prepared by reacting p-hydroxybenzaldehyde with phosphorus oxychloride, then carrying out addition with DOPO (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide), reacting the obtained product with p-aminodiphenylamine, and then carrying out substitution with 3-chloropropyltriethoxysilane; the functional additive is prepared by the following steps: reacting 3, 5-di-tert-butyl-4-hydroxybenzaldehyde with 2-amino-4-methylbenzothiazole, then adding sodium borohydride for reductive amination, substituting the obtained product with cyanuric chloride, and then reacting with N-butyl-2, 2, 6, 6-tetramethyl-4-piperidylamine, and the functional additive is prepared by the following steps: reacting 3, 5-di-tert-butyl-4-hydroxybenzaldehyde with 2-amino-4-methylbenzothiazole; and the protective layer material is endowed with good flame retardance, antibacterial property and long-acting aging resistance.

The invention provides a synthetic method of a novel flame retardant with a phosphaphenanthrene-chloropropyl synergistic structure. The preparation method comprises the following steps: synthesizing bis (1-chloro-2-propyl) phosphoryl chloride from phosphorus oxychloride and epoxypropane in a molar ratio of 1: 2 in a low-temperature condition through a micro-channel reactor, reacting with DOPO-HQ (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-yl-1, 4-benzenediol), adding a specific solvent and a catalyst, reacting to generate a crude product, filtering, washing, carrying out reduced pressure distillation, and recrystallizing to obtain the 2-(1-chloro-2-propyl) phosphoryl chloride, namely the 2-(1-chloro-2-propyl) phosphoryl chloride-DOPO-HQ (9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10-yl-1, 4-benzenediol). The novel flame retardant with the phosphaphenanthrene-chloropropyl synergistic structure is obtained. A phosphaphenanthrene-chloropropyl synergistic structure is designed, so that the molecular weight and the phosphorus content are improved, and the gas-phase flame-retardant and condensed carbon-forming synergistic flame-retardant effect is improved; the thermal stability and the molecular weight are improved through a molecular bridge chain (hydroquinone), and migration is inhibited. The flame retardant has excellent flame retardant property.

The invention provides a preparation process of 2-(p-chlorphenyl)-5-trifluoromethyl-pyrrole-3-nitrile, which comprises the following steps: taking p-chlorphenylglycine and trifluoroacetic acid as raw materials, carrying out acylation reaction under the action of a catalyst to generate 4-(4-chlorphenyl)-2-trifluoromethyl-3-oxazole-5-ketone, then adding 2-chloroacrylonitrile, and carrying out reaction under the action of a catalyst to generate 4-(4-chlorphenyl)-2-trifluoromethyl-3-oxazole-5-ketone. And carrying out cyclization reaction to generate the 2-(p-chlorphenyl)-5-trifluoromethyl-pyrrole-3-nitrile product. According to the method, acylation reagents such as phosphorus trichloride and phosphorus oxychloride are not used, so that the generation of phosphorus-containing and high-ammonia-nitrogen wastewater is reduced, the wastewater treatment difficulty and cost are reduced, and meanwhile, the production risk and the environmental harm are also reduced; the final product is directly prepared by a one-pot method, and the operation of separating and purifying the intermediate product by using another solvent is avoided, so that the steps are greatly simplified, the production efficiency is improved, the use of the solvent can be reduced, and the hidden danger in the solvent recovery process is reduced.

The present invention discloses a preparation method of mesotrione, and the method steps are as follows: S1: Under the protection of an inert gas, 3-chloro-2-methylbenzenemethanethiol, phosphorus oxychloride, a composite catalyst and an organic solvent are mixed and reacted. After the reaction is completed, 2-chloro-3-methyl-4-methylthiophenylaldehyde is obtained through separation and vacuum distillation; 2-chloro-3-methyl-4-methylthiophenylaldehyde is mixed with sodium tungstate dihydrate and methanol, and hydrogen peroxide is added for reaction. After the reaction, 2-chloro-3-methyl-4-methylsulfonylbenzoic acid is obtained through filtration; S2: Preparation of 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid; S3: 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid is mixed and reacted with thionyl chloride and dichloroethane, and the reaction product is further reacted with 1,3-cyclohexanedione, triethylamine and samarium trichloride to prepare mesotrione. The present invention simplifies the preparation route of mesotrione, the preparation process is more green and safe, and the yield of mesotrione is higher.

The invention discloses a preparation method of cinacalcet hydrochloride. The preparation method comprises the following steps: 1) carrying out a reaction on 3-(3-trifluoromethylphenyl) propanol and phosphorus oxychloride; first post-treatment: extracting the product obtained in the step 1) by using an organic solvent, drying and concentrating to obtain 1-(3-chloropropyl)-3-trifluoromethyl benzene; (2) carrying out substitution reaction on the 1-(3-chloropropyl)-3-trifluoromethyl benzene obtained by the first post-treatment and (R)-1-(1-naphthyl) ethylamine; the product obtained in the second step is subjected to extraction, drying and concentration through an organic solvent and then subjected to a salt forming reaction with hydrochloric acid, and cinacalcet hydrochloride is obtained.According to the method, it is guaranteed that the product has the good yield and high purity, meanwhile, the impurity content, especially oxidation impurities, is remarkably reduced, and the appearance color and luster of cinacalcet hydrochloride are effectively improved.

The invention relates to an environment-friendly preparation method of 2-butyl-4-chloro-5-formyl imidazole, which comprises the following steps of: taking 2-butyl-4-chloro-5-formyl imidazole as a raw material; according to the method disclosed by the invention, a small amount of N-chlorosuccinimide is added in the chlorohydroformylation process, so that the effects of activating reaction, reducing the dosage of phosphorus oxychloride and improving the reaction conversion rate are achieved; in the post-treatment process, water replaces an organic solvent, and the pH value and crystallization temperature of the system are reasonably adjusted by utilizing the difference of solubility of 2-butyl-4-chloro-5-formyl imidazole in water with different pH values and different temperatures, so that 2-butyl-4-chloro-5-formyl imidazole in the system is separated out as much as possible, and the purity of 2-butyl-4-chloro-5-formyl imidazole is improved. And the recovery rate of the 2-butyl-4-chloro-5-formyl imidazole and the purity of the finished product are improved. The method disclosed by the invention is a green, environment-friendly and efficient preparation method of the 2-butyl-4-chloro-5-formyl imidazole, and is suitable for being used in the industry.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a preparation method of a cabozantinib intermediate. The invention provides a novel preparation method of a cabozantinib intermediate 6.7-dimethoxy-4-(4-nitrophenoxy) quinoline, which comprises the following steps: by taking 6.7-dimethoxyquinoline-4-alcohol as a starting material, carrying out hydroxyl protection on the 6.7-dimethoxyquinoline-4-alcohol and tert-butyldimethylsilyl chloride, and then reacting with p-fluoronitrobenzene to obtain 6.7-dimethoxy-4-(4-nitrophenoxy) quinoline; the method avoids the problems of serious environmental pollution and strong corrosion to equipment due to the use of highly toxic reagents such as phosphorus oxychloride, sulfonyl chloride and oxalyl chloride in the traditional hydroxyl chlorination, and is suitable for large-scale process production.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a method for synthesizing a cabozantinib intermediate. According to the method, 6, 7-dimethoxyquinoline-4-alcohol is taken as a starting material and reacts with tert-butyl 4-hydroxyphenylcarbamate, then deprotection is carried out, and 6, 7-dimethoxy-4-(4-nitrophenoxy) quinoline is obtained, so that the method avoids the problems that reagents such as highly toxic phosphorus oxychloride, sulfonyl chloride and oxalyl chloride are used during traditional hydroxyl chlorination, the environment is seriously polluted, the cost is low, and the like. And the method is suitable for large-scale production.

The invention discloses a green synthesis process of 2-amino-3-chloro-5-trifluoromethylpyridine, and belongs to the technical field of preparation of pesticide intermediates. The method comprises the following steps: by taking 3, 5-dichloropyridine as a raw material, carrying out nitrogen-oxidation reaction; then carrying out trifluoromethylation reaction under the action of a palladium catalyst; then carrying out chlorination reaction on phosphorus oxychloride; and finally, carrying out ammonification reaction to generate the 2-amino-3-chloro-5-trifluoromethylpyridine. According to the method, all the raw materials can be conveniently purchased on the market, the process of each step of reaction is simple and convenient, chloropyridine is directly subjected to trifluoromethylation by adopting trifluoromethyl potassium trifluoroborate and a palladium catalyst, the reaction yield is high, and industrial production is easy; meanwhile, a by-product ammonia chloride generated in the mother liquor in the amino substitution step can be recycled as a by-product.

The utility model discloses a device for preparing 5-fluoro-4, 6-dichloropyrimidine, which comprises a head tank, a reaction kettle, a rectifying tower, a condenser, a vacuum pump, a first receiving tank, a second receiving tank and a third receiving tank, a feed port of the head tank is used for receiving dichloroethane and phosphorus oxychloride, and a discharge port of the head tank is connected with a first feed port of the reaction kettle; the reaction kettle is further provided with a feeding port used for feeding dihydroxypyrimidine, a discharging port of the reaction kettle is connected with a feeding port of the rectifying tower, the rectifying tower is connected with a condenser, and the condenser is connected with a vacuum pump. A discharging port of the rectifying tower is connected with a feeding port of a first receiving tank, a feeding port of a second receiving tank and a feeding port of a third receiving tank through a first pipeline, a second pipeline and a third pipeline respectively, and valves are arranged on the first pipeline, the second pipeline and the third pipeline respectively. A vacuum port of the first receiving tank, a vacuum port of the second receiving tank and a vacuum port of the third receiving tank are respectively connected with a vacuum pump.

The invention belongs to the field of pesticide chemicals, and in particular to a kind of synthetic method of acephate. Phosphorus oxychloride and methanol generate methyl dichlorophosphate through substitution reaction, methyl dichlorophosphate and ammonia generate methylphosphoramide chloride through acylation reaction, methylphosphoramide chloride and methyl mercaptan obtain methylamidophos through substitution reaction, and methylamidophos and acetic anhydride generate acephate through acylation reaction. Using phosphorus oxychloride as raw material, by multiple substitution reactions and one-step acylation reaction, target product can be obtained, avoiding the reaction of phosphorus trichloride and sulfur under high temperature conditions and the isomerization reaction of O, O-dimethylthiophosphoramide, and the use of caustic alkali. Meanwhile, the product appearance properties prepared by the inventive method are good.

The invention discloses a copper smelting acid mist eliminating reagent, and relates to the technical field of copper smelting, the reagent is a compound synthesized by taking perfluoroalkyl ethyl alcohol as a raw material, fatty alcohol-polyoxyethylene ether and phosphorus oxychloride, n can be 4 or 6, and represents perfluorobutyl ethyl alcohol and perfluorohexyl ethyl alcohol, and n represents 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 13, 14, 16, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17, 17 m is 6-14 and represents a group of polyoxyethylene ether with the polymerization degree of 6-14, R is C4-C12 fatty alcohol and comprises straight-chain alcohol and branched-chain alcohol, M is an organic matter containing a basic group and is used for neutralizing the acidity of phosphoric acid, one of alanine, arginine, serine, triethanolamine and-amino-2-methyl-1-propanol can be adopted, and n is an integer of 1-3. According to the copper smelting acid mist eliminating reagent, by adopting the reagent provided by the invention, acid mist can be effectively inhibited in a non-ferrous metal electrodeposition process, a relatively good inhibition effect on the acid mist is achieved, and compared with an existing reagent, the reagent has the advantages of being good in acid mist inhibition effect, low in cost and relatively low in price.

The invention discloses a creatine phosphate sodium continuous flow synthesis process, which comprises the following steps: adding a proper amount of dichloromethane and a proper amount of creatinine into a storage tank A, and stirring until the solution is clear to obtain a storage tank A material; adding a proper amount of phosphorus oxychloride into a storage tank B to obtain a storage tank B material; conveying the materials in the storage tank A and the storage tank B into a micro-channel reactor, reacting to obtain a dichlorophosphoric acid creatinine reaction solution, then concentrating in a concentration kettle, adding methylbenzene, stirring, crystallizing, and filtering to remove residual phosphorus oxychloride; adding a proper amount of purified water and sodium hydroxide into a tank D, stirring until the solution is clear to obtain a storage tank D material, adding the materials in the tank C and the tank D into a micro-channel reactor, reacting to obtain a creatine phosphate sodium solution, transferring the solution into an extraction layering kettle, standing and layering to obtain an upper water layer, and filtering the upper water layer to obtain the creatine phosphate sodium. And adding activated cationic resin, stirring, filtering by using a microfiltration membrane when the pH value of the feed liquid is reduced to 9-10, and crystallizing by adding 95% ethanol into the filtrate to obtain the creatine phosphate sodium finished product. Through a continuous flow synthesis process, the use and residue of phosphorus oxychloride are reduced, and the product safety is improved; reaction impurities and phosphate residues are reduced, the reaction efficiency is improved, and the cost is reduced.

The invention relates to a hyperbranched intumescent flame retardant / co-curing agent and a preparation method thereof as well as flame-retardant modified epoxy resin and application thereof, and the hyperbranched intumescent flame retardant / co-curing agent is prepared by taking 3-amino-1, 2-propylene glycol, triethylamine, cyanuric chloride, phosphorus oxychloride and organic polyamine as raw materials through a three-step substitution reaction. On one hand, the flame retardant has various flame-retardant structures such as triazine and phosphate, belongs to a single-molecule intumescent flame retardant, and has an excellent flame-retardant effect due to mutual synergism of different flame-retardant structures; and on the other hand, the flame retardant has a polyamine structure and a hyperbranched structure which can participate in an epoxy curing reaction, the polyamine structure can enable flame retardant molecules to be stably distributed in an epoxy resin material in a covalent bond manner, and the hyperbranched structure can endow the epoxy resin material with good mechanical properties. Limit oxygen index (LOI), vertical combustion UL-94 and mechanical property test results show that the flame retardant shows excellent flame retardance and impact resistance, and the problem that flame retardance and other comprehensive properties of an epoxy resin material are difficult to consider can be solved.

The application provides a preparation method of bosentan, which comprises the following steps: mixing phosphorus oxychloride and 5-(2-methoxyphenoxy)-[2,2'-bipyrimidine]-4,6(1H,5H)-dione, reacting to obtain 4,6-dichloro-5-(2-methoxyphenoxy)-2,2'-bipyrimidine; then mixing the 4,6-dichloro-5-(2-methoxyphenoxy)-2,2'-bipyrimidine with 4-tert-butylbenzenesulfonamide, an acid binding agent and a polar aprotic solvent, and reacting to obtain 4-tert-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide potassium salt; then mixing the 4-tert-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-4-pyrimidinyl]benzenesulfonamide potassium salt with ethylene glycol, an alkali metal hydroxide and tetrahydrofuran to obtain a bosentan precursor; and finally mixing the bosentan precursor with ethanol and water, reacting, cooling and crystallizing to obtain bosentan. The preparation method of bosentan can greatly save reaction time, improve reaction yield, reduce impurity content, simplify post-treatment operation, reduce preparation cost and be convenient for industrial large-scale production and application.

The application discloses a method for producing berberine by using recycled formic acid, and belongs to the technical field of preparation of medical chemical raw materials. The method comprises the following steps: 1, adding diatomite powder to a dilute hydrochloric acid solution to remove impurities, and preparing a water removing agent by acid pickling, roasting and dropwise adding phosphorus oxychloride; 2, adding anhydrous sodium sulfate to crude formic acid to pre-dehydrate, adding the water removing agent to remove water after filtering out the precipitate, and obtaining refined recycled formic acid; 3, adding copper chloride, refined recycled formic acid, N-2,3-dimethoxybenzyl piperidyl ethylamine hydrochloride into a reactor, dropwise adding 40% glyoxal, and performing cyclization reaction for 3-4 hours; 4, removing the cyclization mother liquor by suction filtration, retaining the solid, adjusting the alkali and heating, filtering out the precipitate and retaining the filtrate, adjusting the acid, cooling and crystallizing, filtering and retaining the solid, rinsing and drying, and obtaining berberine. The application realizes preparation of berberine by using recycled formic acid, and the production process is safe, and the product has high purity and high yield.

The invention discloses an esterification kettle for oxadiazon herbicide production, and belongs to the field of reaction kettle devices. The esterification kettle comprises a lower kettle body, a cooling jacket is arranged on the outer surface of the lower kettle body, and an annular cooling cavity internally provided with a cooling coil is formed by the cooling jacket and the lower kettle body; the bottom and the top of the cooling jacket are respectively communicated with a water inlet pipe and a water outlet pipe; the top and the bottom of the cooling coil are respectively communicated with a water inlet joint and a water outlet joint; the water inlet pipe and the water outlet pipe are respectively communicated with the outlet end and the inlet end of the circulating oil supply mechanism; and the water inlet joint is communicated with the cooling water supply mechanism. The heat conduction oil circulating system and the independent cooling coil pipe are integrated in the annular cooling cavity on the outer side of the lower kettle body, heat conduction oil is responsible for stably removing basic heat in a large area, the built-in cooling coil pipe can provide stronger and quicker local cooling capacity, and when instantaneous temperature rise is caused by violent heat release of phosphorus oxychloride and dichlorophenol, the heat conduction oil circulating system and the independent cooling coil pipe can be rapidly cooled. The cooling coil is used for improving the cooling effect on the top of the reaction system.

The present invention discloses a synthesis method for the menin inhibitor SNDX-5613 (Revumenib) and an intermediate compound thereof. The synthesis method of the present invention has high yield, low cost, avoids the use of phosphorus oxychloride, and improves safety.

The invention discloses a method for selective nitration of naphthylamine through palladium catalysis, 8-nitro-1-naphthylamine and a derivative of 8-nitro-1-naphthylamine, and belongs to the technical field of organic synthesis. Wherein R1 is H, a halogen element, a nitro group, a C1-C4 alkyl group, an acetamido group, an aryl group, an alkoxycarbonyl group, a benzyloxy group or a C1-C4 alkoxy group; the preparation method comprises the following steps: S1, adding a solvent into 2-picolinic acid and a compound as shown in a formula (IV), then adding alkali to adjust the pH value, cooling, then slowly dropwise adding phosphorus oxychloride, magnetically stirring while dropwise adding, heating to room temperature after dropwise adding is completed, and continuing stirring reaction to obtain a compound as shown in a formula (V); and S2, carrying out nitration reaction on the compound as shown in the formula (V) obtained in the step S1 and N-(o-tolyl) quinoline-2-formamide under the action of a silver nitrite and palladium catalyst, and magnetically stirring to obtain a compound as shown in a formula (II). The method is mild in reaction condition and excellent in yield and regioselectivity, and the reaction substrate has good functional group tolerance.

The present invention provides a bosentan preparation method, which comprises: mixing phosphorus oxychloride and 5-(2-methoxyphenoxy)-[2, 2 '-dipyrimidine]-4, 6 (1H, 5H)-diketone, and carrying out a reaction to obtain 4, 6-dichloro-5-(2-methoxyphenoxy)-2, 2'-dipyrimidine, and carrying out a reaction to obtain 4, 6-dichloro-5-(2-methoxyphenoxy)-2, 2 '-dipyrimidine, mixing the N-[6-chloro-5-(2-methoxyphenoxy)-4-pyrimidyl] benzenesulfonamide with 4-tert-butyl benzenesulfonamide, an acid-binding agent and a polar aprotic solvent, and carrying out a reaction to obtain 4-tert-butyl-N-[6-chloro-5-(2-methoxyphenoxy)-4-pyrimidyl] benzenesulfonamide potassium salt; then mixing the bosentan precursor with ethylene glycol, alkali metal hydroxide and tetrahydrofuran to obtain a bosentan precursor; and finally, mixing with ethanol and water, reacting, cooling and crystallizing to obtain bosentan. According to the preparation method of bosentan, the reaction time can be greatly saved, the reaction yield can be improved, the impurity content can be reduced, the post-treatment operation can be simplified, the preparation cost can be reduced, and industrial large-scale production and application can be facilitated.

The invention belongs to the technical field of organic synthesis, and particularly relates to a 2-chloro-4, 6-dimethyl pyrimidine synthesis process, which comprises: 1) mixing 2-hydroxy-4, 6-dimethyl pyrimidine, xylene and phosphorus oxychloride, heating to a temperature of 50-60 DEG C, dropwise adding N, N-diisopropylethylamine, heating to a temperature of 80-105 DEG C after the dropwise adding is completed, carrying out a reaction for 2-3 h, removing excess phosphorus oxychloride, cooling to a room temperature, and carrying out a reaction for 2-3 h to obtain a 2-chloro-4, 6-dimethyl pyrimidine intermediate; a reaction liquid crude product is obtained; and 2) dropwise adding the crude product of the reaction liquid into a supersaturated sodium bicarbonate aqueous solution at 5-15 DEG C, keeping the water temperature in the dropwise adding process, keeping the water temperature after dropwise adding, stirring for 15-35 minutes, filtering, standing and layering filtrate, drying an organic phase by anhydrous magnesium sulfate, removing xylene, and performing reduced pressure distillation to obtain the 2-chloro-4, 6-dimethyl pyrimidine. According to the method, the dosage of phosphorus oxychloride can be reduced, hydrolysis of the product is effectively avoided, the yield of the product is improved, and the method has no obvious amplification effect and is suitable for industrial production.