48 results about "Chlorethoxyfos" patented technology

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 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.