47 results about "Chlorethoxyfos" patented technology

The invention discloses a 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compound as well as a preparation method and application of the 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compound, wherein the compound structure is shown as the following general formula (I). A series of novel 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compounds are synthesized by using 2,3,4-trihydroxy benzoic acid, dimethyl sulfate, diethyl sulfate, methanol, sulfuric acid, nitric acid, hydrogen gas, formamide, phosphorus oxychloride, N-Boc piperazine, hydrochloric acid, aryl sulfonyl chloride and 4-aromatic (benzyl, pyridine and morpholine propyl) substituted piperazine as raw materials through multiple steps. The compound has a better anticancer effect and a plant fungus inhibition effect and can be used for preparing anticancer medicine and plant fungus resistance pesticide. (I) is shown as the accompanying drawing.

The invention discloses a preparation method of halogen-free intrinsic flame-retardant waterborne polyurethane. The preparation method comprises the following steps: firstly, performing a reaction onphosphorus oxychloride with pentaerythritol to prepare an intermediate product with a diphosphoryl chloride functional group; performing a reaction on the intermediate product with diglycolamine and other substances, thereby preparing a micromolecular flame retardant containing phosphorus and nitrogen flame-retardant elements, and finally performing a reaction on the micromolecular flame retardantserving as a hard segment chain extender with polyether polyol, isophorone diisocyanate, 2,2-dimethylolpropionic acid and other substances to prepare the halogen-free intrinsic flame-retardant waterborne polyurethane. According to the invention, the reactive halogen-free intrinsic flame-retardant waterborne polyurethane is prepared by taking the halogen-free flame retardant as a reaction substance, so that the product is good in flame-retardant effect, simple in synthesis method and relatively low in cost, has very good practicability and economy, and has a good market prospect.

The invention relates to a synthesis method of 8-nitro-2-tetrazol-5-yl-4-oxo-4H-1-benzopyran. The method comprises the following steps: firstly nitrifying hydroxyacetophenone taken as a starting material with a nitric acid so as to generate a mixture of 2-hydroxy-3-nitroacetophenone and 2-hydroxy-5-nitroacetophenone; salifying the mixture by using an inorganic base, carrying out separation and purification and then hydrolyzing with an acid so as to obtain 2-hydroxy-3-nitroacetophenone (A-2); carrying out a cyclization reaction on the 2-hydroxy-3-nitroacetophenone (A-2) and ethyl cyanoformate so as to generate 8-nirto-2-cyano-4-oxo-4H-1-benzopyran (A-3); and finally, reacting with sodium azide so as to generate the 8-nitro-2-tetrazol-5-yl-4-oxo-4H-1-benzopyran (A-6). According to the method, phosphorus oxychloride with an application risk and large pollution and an ammonia gas with strong stimulating smell are not used, so that the production is safe and environment-friendly; and the generation of waste gases is reduced at the same time, so that the synthesis process is shortened. Thus, the operation is simplified; the production cost is lowered; and the 8-nitro-2-tetrazol-5-yl-4-oxo-4H-1-benzopyran is high in purity.

The invention relates to the technical field of drug synthesis, and provides a method for synthesizing 2-fluoro-5-trifluoromethylpyrimidine. The invention uses 5-methyluracil as a raw material, and obtains the target product through a cyclic chlorination reaction, a reduction reaction, a chlorination reaction and a fluorination reaction, the process is simple, the raw materials are cheap and easy to obtain, the yield is high, and no generation of Heavy metal pollution; and the present invention uses phosphorus oxychloride to perform chlorination in the cyclic chlorination reaction, and uses chlorine to perform chlorination in the chlorination reaction, and the costs of both are relatively low, and phosphorus pentachloride is used in the cyclic chlorination reaction. Recovering phosphorus oxychloride can further reduce the reaction cost.

The invention provides a synthetic method for cyclophosphoramide. According to the synthetic method, phosphorus oxychloride is slowly added into a mixed solution of dichloroethane, polyphosphoric acidand acetic anhydride, 3-amino propyl alcohol is dropwise added so as to prepare 2-chloro-2-oxo-[1.3.2] oxygen-nitrogen-phosphorus heterocyclic hexane; and dichloroethane and a 5a molecular sieve areadded, ammonia gas is introduced, heating is carried out at 4 atm to reach 120 DEG C, reaction is carried out for 2-2.5 hours, and treatment is carried out so as to obtain the cyclophosphoramide. Themethod has the advantages that the reaction conditions are relatively mild, and the yield and the content are high.

The invention belongs to the technical field of medicine chemosynthesis, and relates to a preparation method of 6-chloro-3-methyluracil. The method comprises the following steps that 1, methylurea, anorganic solvent and alkali are added into a reaction container for stirring and dissolution, then malonic acid or malonic ester is added, heating and reflux are conducted, then cooling is conducted,acid is added to adjust a pH value of reaction liquid, water is added, the reaction liquid is cooled, suction filtration is conducted, and drying is conducted to obtain a white to off-white first intermittent in a shape of loose powder; 2, phosphorus oxychloride is used for chloridizing the first intermittent to obtain a crude product; 3, the crude product prepared in the step 2 is subjected to decoloration by means of activated carbon to obtain a finished product. According to the preparation method of the 6-chloro-3-methyluracil, the product in the step 1 precipitates in a form of sodium salt, that is to say, the first intermittent is 1-sodium methylbarbiturate, compared with the prior art where a first intermittent precipitates in a form of 1-methylbarbituric acid, the preparation method of the 6-chloro-3-methyluracil has the advantages that the yield is obviously improved, moreover, in the step 2, acetonitrile is used as the solvent, the phosphorus oxychloride usage is reduced, post-treatment is convenient, and meanwhile, the product has a good crystal form, and is easy to filter.

The invention relates to a phosphorus-nitrogen-silicon intumescent flame retardant containing a triazine ring and a cage structure and a synthesis method of the intumescent flame retardant. The synthesis method comprises the steps as follows: a solvent is added to a container, phosphorus oxychloride is added and stirred to be dispersed, PEPA (1-oxy phospha-4-(hydroxymethyl)-2,6,7-trioxabicyclo[2.2.2]octane) and an acid-binding agent are dropwise added step by step, and a PEPA-containing unitary substituent is obtained; substances with diamine or dihydric alcohol are added to the other container and mixed with the solvent and the acid-binding agent, the PEPA-containing unitary substituent is slowly dropwise added, and a phosphorous-containing diamine intermediate is obtained after separation; the solvent is added to a container provided with a reflux condenser and the like, cyanuric chloride is added and stirred to be dispersed, an amino silane coupling agent and the acid-binding agent are dropwise added step by step, and a silicon-containing unitary substituent is obtained; the mixture of the phosphorous-containing diamine intermediate and the acid-binding agent is slowly dropwise added, cooling, washing and drying are performed, and a powdery solid, namely, the phosphorus-nitrogen-silicon intumescent flame retardant containing the triazine ring and the cage structure, is obtained. The phosphorus-nitrogen-silicon intumescent flame retardant has the advantages that the flame retardant has certain polymerization degree, high molecular weight, higher charcoal forming amount and better thermal stability, the proportion of acid sources, carbon sources and gas sources in molecular structures is relatively proper and the like.

The invention discloses a 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compound as well as a preparation method and application of the 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compound, wherein the compound structure is shown as the following general formula (I). A series of novel 4-(4-substituted piperazine)-5,6,7-trialkoxy quinazoline type compounds are synthesized by using 2,3,4-trihydroxy benzoic acid, dimethyl sulfate, diethyl sulfate, methanol, sulfuric acid, nitric acid, hydrogen gas, formamide, phosphorus oxychloride, N-Boc piperazine, hydrochloric acid, aryl sulfonyl chloride and 4-aromatic (benzyl, pyridine and morpholine propyl) substituted piperazine as raw materials through multiple steps. The compound has a better anticancer effect and a plant fungus inhibition effect and can be used for preparing anticancer medicine and plant fungus resistance pesticide. (I) is shown as the accompanying drawing.

The invention discloses a separation and purification process of a byproduct 2-butoxyethyl chloride in the production process of tris (butoxyethyl) phosphate, which comprises the following steps of: adding titanium tetrachloride into recycled ethylene glycol monobutyl ether containing 2-butoxyethyl chloride with the concentration of more than or equal to 30%, completely dissolving, cooling, dropwise adding excessive phosphorus oxychloride, and reacting at the temperature of between 20 and 30 DEG C to obtain the 2-butoxyethyl phosphate. After dropwise adding is completed, heat preservation is conducted for a period of time, heating continues, ethylene glycol monobutyl ether in the materials is thoroughly reacted to obtain butoxyphosphoric acid diacyl chloride, reduced pressure distillation is conducted, a 2-butoxychloroethane crude product and a base material are separated out, the base material is used for preparing TBEP, liquid caustic soda and water are added into the 2-butoxychloroethane crude product, stirring alkali washing is conducted, and the 2-butoxychloroethane crude product is obtained. And standing to separate out a discharge layer and an alkali washing wastewater layer, adding water into the separated discharge layer, stirring and washing, standing, and separating out a 2-butoxychloroethane finished product and washing wastewater. The method disclosed by the invention is tightly combined with a tris (butoxyethyl) phosphate production process, and ethylene glycol monobutyl ether is intermittently and intensively treated and recycled by using the existing equipment.

The invention provides a preparation method of mepanipyrim and belongs to the field of pesticide chemical synthesis technologies. The preparation method of the mepanipyrim comprises the following steps: firstly, reacting phenyl guanidine salt with ethyl acetoacetate so as to prepare phenylamino pyrimidone, reacting the phenylamino pyrimidone with phosphorus oxychloride so as to prepare 2-chloro-pyrimidine phenylamine; subsequently, carrying out coupling and crossing reaction between the 2-chloro-pyrimidine phenylamine and alkyne so as to prepare mepanipyrim. The preparation method of mepanipyrim has the advantages that the used raw materials and reagents are cheap and easily available; the reaction process is simple, the reaction conditions are mild, the cost is low, the yield is high, a good condition is created for industrial large-scale production and commercialization of the products.

The invention discloses a purification method for salifying 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline. The method comprises the following steps: allowing N-(2-cyclohexenyl ethyl)-2-(4-methoxyphenyl) acetamide to react with phosphorus oxychloride in xylene to obtain 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline, carrying out reduced pressure evaporation to remove xylene and excessive phosphorus oxychloride, and adding a solvent with destroyed phosphorus oxychloride to destroy residual phosphorus oxychloride; and extracting the 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline hydrochloride by using halogenated hydrocarbon, carrying out vacuum concentration to remove the solvent, adding a crystallization solvent, and crystallizing to obtain the high-purity 1-(4-methoxybenzyl)-3, 4, 5, 6, 7, 8-hexahydroisoquinoline hydrochloride. The method is convenient and safe in process and high in yield, the content of the arylation compound impurity 1-(4-methoxybenzyl)-5, 6, 7, 8-tetrahydroisoquinoline is low, the amount of three wastes is small, and the method is suitable for industrial production.

The invention relates to an synthesizing method of 2-methyl-7-( substituted pyrimidine-4-amino)-4-(substituted piperazine-1-base) piperidine-1-base) isoindoline-1-ketone and an intermediate thereof, mainly solving the technical problems of overlength single-line synthetic route, difficult separation and purification, low productivity, high synthesizing cost, narrow applicability, and the like of the traditional synthesizing method. The process method comprises the following steps of: carrying out substitution reaction on 2,4,5-trichloropyrimidine as a raw material and sodium methyl mercaptideto generate the intermediate, i.e. 2,5-dichloro-4-methylthiopyrimidine; then carrying out the substitution reaction with aromatic amine to generate the intermediate, i.e. 2-aromatic amino-4-methylthio-5-chloropyrimidine; then hydrolyzing the methylthio to generate the intermediate, i.e. 2-aromatic amino-4-hydroxy-5-chloropyrimidine; enabling a hydroxyl compound to generate dichloride under the action of phosphorus oxychloride; and finally carrying out the substitution reaction with amine to obtain the 2-methyl-7-(5-chlorine-2-aromatic amido-pyrimidine-4-amino)-4-(4-(4-methyl piperazine-1-base) piperidine-1-base) isoindoline-1-ketone under the action of hydrogen chloride ethyl acetate.

The invention discloses a high flame-retardant art paint, which is composed of the following raw materials in parts by weight: 10-50 parts by weight of acrylic acid copolymer; 0.1-5 parts by weight of rheological additive; 0.1-0.6 parts by weight of dispersant; ‑0.6 parts by weight; 2‑10 parts by weight of film-forming aids; 1‑5 parts by weight of antifreeze; 0.1‑0.5 parts by weight of defoamers; 0.1‑0.3 parts by weight of preservatives; PH regulator 0.1-0.8 parts by weight; water 1-40 parts by weight; filler 10-30 parts by weight; pearlescent effect of 10-20 parts by weight; 100-150 parts of oxygen compound monomer, 2-5 parts of starter, 5-20 parts of flame retardant catalyst; the halogen-containing epoxy compound monomer is selected from 4,4,4-trichloro-1,2-ring One or more of oxybutane, 4,4,4,-tribromo-1,2-epoxybutane or epichlorohydrin; the flame retardant catalyst is selected from phosphorus oxychloride, dioxypentoxide One or more of antimony and tetrakis hydroxymethyl phosphorus chloride; the initiator is selected from propylene glycol. The invention has excellent scratch resistance, high hardness, good hand feeling and strong layering.