285 results about "Phosphorus pentachloride" patented technology

The invention discloses a method for preparing aromatic dimethyl chloride, which relates to the technical field of preparation methods of aromatic chloride. The method comprises the following steps of: reacting aromatic dioctyl phthalate with a chlorinating agent to generate the aromatic dimethyl chloride; evaporating the chlorinating agent; exhausting tail gas; and distilling the obtained aromatic dimethyl chloride, wherein the reaction of the aromatic dioctyl phthalate and the chlorinating agent is performed in the presence of a catalyst, namely pyridine or N-methyl pyrolidone; and the chlorinating agent is one or more of chlorine, phosphorus trichloride, phosphorus pentachloride and thionyl chloride. Compared with the prior art, the method for preparing the aromatic dimethyl chloride has the advantages that: the yield and the purity of the aromatic dimethyl chloride are increased, transformation rate is up to 95 percent, and the purity is up to 99.9 percent.

The invention relates to a method for synthesizing p-acetamido benzene sulfonyl chloride by phosphorus pentachloride, relating to the preparation method for sterilization and mould inhibition midbody of sulfonamides. The invention takes acetanilide and chlorosulfonic acid as raw materials, uses phosphorus pentachloride as chlorinating agent; under the action of organic dissolvent, the raw materials are sulfonated, chloridized, separated, and washed to obtain the product. The invention has the effects of little chlorosulfonic acid usage, high product yield, few generated waste acid,, completely cycling dissolvent, recycled by-products, low manufacturing cost, being convenient to popularize and apply, and the like. The products prepared by the method can be widely applied to the preparation of the sterilization and mould inhibition of sulfonamides and industries such as coating, plastics, pesticides, etc.

The invention discloses a green synthesis method of methyl phosphorus dichloride. The method comprises the following steps: by taking phosphorus pentachloride as a catalyst, heating phosphorus trichloride and phosphorus pentachloride into vapor, and preheating to 150-250 DEG C and mixing with methane and then entering a tubular reactor, and reacting for 0.1-1.0s under the conditions that the temperature is at 400-500 DEG C and the pressure is 0.3-1.2MPa, to obtain methyl phosphorus dichloride. After the catalyst is applied to methane and phosphorus trichloride to synthesize methyl phosphorus dichloride, the conversion rate of the phosphorus trichloride is effectively improved to 40%-50%, and the yield is 90%-95%; the adopted catalyst phosphorus pentachloride is decomposed into phosphorus trichloride and chlorine gas, the catalyst and the product is not required for separation, three wastes are not generated during the whole preparation, and all the materials are recycled, so that the resources are saved, the environment is beneficially protected, and the synthesis method is green.

The invention discloses a method for effectively preparing cylopropyl ethylnen as shown in the formula (I). The method comprises the steps that firstly, cylopropyl methyl ketone shown in the formula (II) is taken as a raw material and fully reacts in an organic solvent under the effect of phosphorus pentachloride and a catalyst, a reaction solution is subjected to reduced pressure distillation to obtain 1,1-dichloro-1-cylopropyl ethane as shown in the formula (III), an elimination reaction is then carried out under the effect of alkali, and a reaction solution is subjected to rectification and purification to obtain the product cylopropyl ethylnen. The method for effectively preparing the cylopropyl ethylnen has the advantages of being mild in reaction condition, high in yield, low in cost, little in three-waste and the like, and is suitable for industrial production.

The invention discloses a method for preparing antithrombotic medicament apixaban. The method comprises the following steps of: obtaining a compound V by performing an amidation-cyclization two-step one-pot reaction on paranitroaniline serving as a raw material and a general purpose reagent 5-chlorine valeryl chloride under an alkaline condition; performing di-chlorination on the alpha-hydrogen of the V by using phosphorus pentachloride; performing a condensation-elimination reaction with excess morpholine to obtain a compound VI; reducing the VI into a compound VII by using sodium sulfide; performing the amidation-cyclization two-step one-pot reaction on the VII and the 5-chlorine valeryl chloride to obtain a key intermediate III; obtaining II by performing a [3+2] cyclization-elimination reaction on the III and another intermediate IV; and finally, obtaining I by performing aminolysis on the II. The method has the advantages that: process design is reasonable, expensive reagent is not used, reaction yield is high, raw material cost is low, and the method is simple and convenient to operate, has no harsh reaction condition, and is easy to perform large-scale production.

The invention discloses a preparation method of intermediate cyclopropyl acetylene of anti-AIDS (acquired immune deficiency syndrome) drug efavirenz. The preparation method comprises the steps of performing a reaction in an organic solvent by taking cyclopropyl methyl ketone as a raw material and phosphorus pentachloride as a chlorinating agent by the action of a catalyst to generate alpha, alpha-dichloroethyl cyclopropane and phosphorus oxychloride, performing decompressed rectification to remove phosphorus oxychloride, removing part of hydrogen chloride from alpha, alpha-dichloroethyl cyclopropane by the action of triethylamine to generate alpha-chlorovinyl cyclopropane, and further removing part of hydrogen chloride by the action of strong base to generate cyclopropyl acetylene. Phosphorus oxychloride is removed by the decompressed rectification; the generation of much phosphorus wastewater due to hydrolysis of phosphorus oxychloride in ice water is avoided; recovered phosphorus oxychloride can be comprehensively utilized by simple rectification; waste gas, wastewater and industrial residue are reduced; the cost is lowered; cyclopropyl acetylene is prepared from alpha-chlorovinyl cyclopropane via a reaction rectification technology; and the method has the advantages of high conversion rate, good selectivity, low energy consumption and the like, and is suitable for industrialproduction.

The invention provides a preparation method of a lithium hexafluorophosphate, which comprises the following steps: firstly, reacting a phosphorus pentachloride with an anhydrous hydrogen fluoride to form mixed liquid of the phosphorus pentachloride and the anhydrous hydrogen fluoride; secondly, preparing anhydrous hydrogen fluoride solution of lithium fluoride; and finally, adding the anhydrous hydrogen fluoride solution of the lithium fluoride into the mixed liquid of the phosphorus pentachloride and the anhydrous hydrogen fluoride, and sequentially performing reaction, crystallization, separation and drying to obtain a pure lithium hexafluorophosphate product. The preparation method of the invention has the advantages of mild reaction, high safety and purity of the lithium hexafluorophosphate product of over 99.9 percent; and the mother liquor can be reclaimed and reused so that the cost is reduced.

The invention discloses a method for catalytically synthesizing hexachlorocyclotriphosphazene. The method is characterized by comprising the following steps: taking raw materials according to a molar ratio that quaternary ammonium salt:anhydrous metal chloride:chlorobenzene:ammonium chloride:phosphorus pentachloride is 1-2:0.1-1:5-10:1-1.4:1; adding the quaternary ammonium salt and anhydrous metal chloride into a reactor to react by stirring for 1 to 2 hours at a temperature of between 80 and 120 DEG C to prepare ionic liquid; adding the chlorobenzene, the ammonium chloride and the phosphorus pentachloride into the reactor to react by stirring for 1 to 5 hours at a temperature of between 100 and 130 DEG C to obtain reaction mixed material; separating or / and filtering the reaction mixed material to separate the ionic liquid from chlorobenzene solution containing the reactant; and washing and distilling the chlorobenzene solution containing the reactant at reduced pressure to obtain the hexachlorocyclotriphosphazene product. The method has simple and safe operation and low cost, and is easy for industrial production and application.

A preparation method of phosphorus pentafluoride gas comprises a step of causing phosphorus pentachloride to react with anhydrous hydrogen fluoride, wherein, the reaction occurs in the presence of a solvent. A preparation method of lithium hexaflourophosphate comprises a contact reaction between solid lithium fluoride and phosphorus pentafluoride gas, wherein the phosphorus pentafluoride gas is prepared by the method of the invention. Compared with the preparation method of the lithium hexaflourophosphate with the phosphorus pentafluoride gas as the raw material in the prior art, the phosphorus pentafluoride gas prepared by the preparation method of the invention has higher purity and lower cost. The yield of the lithium hexaflourophosphate prepared by the method of the invention is higher than 93%, and the purity thereof is up to 99.95%.

The invention discloses a preparation method of a phosphonitrile chloride catalyst, and an application of the phosphonitrile chloride catalyst in the preparation of alkoxy-terminated polysiloxane. Thepreparation method comprises the following steps: purging a reaction device with nitrogen to achieve preheating treatment, opening the reaction device to remove condensate water, and sequentially infiltrating the reaction device with dichloromethane and tetrachloroethane; mixing and uniformly stirring tetrachloroethane and ammonium chloride to prepare a tetrachloroethane solution of ammonium chloride for later use; adding phosphorus pentachloride into the reaction device, slowly raising the temperature to 140-160 DEG C under the protection of nitrogen, then dropwise adding the prepared tetrachloroethane solution of ammonium chloride, carrying out a reflux reaction after the drop-by-drop addition is completed, then raising the temperature to 170-175 DEG C, continuously carrying out the reflux reaction, and cooling the reaction device to room temperature after the reaction is completed; and adding anisole into the reaction solution, and performing stirring under a vacuum condition to achieve uniform mixing in order to obtain target crystals which are the phosphonitrile chloride. The prepared phosphonitrile chloride has a high catalytic activity; and when the phosphonitrile chlorideis used for preparing alkoxy-terminated polysiloxane, a polymer with an excellent storage stability can be effectively prepared.