32 results about "Phosphorous pentachloride" patented technology

The invention relates to a 5-fluctyosine preparation method suitable for industrial production, belonging to the technical field of pharmaceutical chemical synthesis. The method comprises the following steps: by using 2-methoxy-5-fluorouracil as a raw material, chlorinating with phosphorous pentachloride to obtain 2-methoxy-4-chloro-5-fluoropyrimidine, and concentrating the acidic water phase obtained by after-treatment for later use; carrying out amination reaction on the 2-methoxy-4-chloro-5-fluoropyrimidine and an aminating agent to obtain 2-methoxy-4-amido-5-fluoropyrimidine; and carrying out acidic hydrolysis on the 2-methoxy-4-amido-5-fluoropyrimidine by using the concentrated acidic water phase recycled from chlorination to obtain the 5-fluctyosine. The 5-fluctyosine preparation method provided by the invention has the advantages of high yield, convenient after-treatment and fewer three-waste pollutants, solves the problems of high virulent product consumption, difficulty in acidic waste gas treatment, high pollution, high cost and the like in the traditional technique, and is suitable for industrial production application. The total mole yield is up to 70% or above.

The invention belongs to the field of medicine, and in particular relates to a preparation method of eplerenone. Starting from 17α-pregna-4-ene-7α, 21-dicarboxylic acid-11α, 17β-dihydroxy-3-oxo-γ-lactone-7-methyl ester as starting materials, phosphorus pentachloride and Dehydration reaction occurs under the action of boron trihalide to obtain 17α-pregna-4,9(11)-diene-7α, 21-dicarboxylic acid-17β-hydroxy-3-oxo-γ-lactone, 7- Methyl ester, 17α-pregna-4,9(11)-diene-7α, 21-dicarboxylic acid-17β-hydroxy-3-oxo-γ-lactone, 7-methyl ester obtained by epoxidation Eplerenone. The preparation method has specificity, reduces the generation of impurities, and the obtained product has good quality and high yield, and the product purity reaches over 99.5%. The raw material is easy to obtain, the operation is simple, the reaction condition is mild, and industrial production is easy to realize.

The invention discloses an internal circulation reactor and method for continuously preparing phosphorus pentafluoride. The internal circulation reactor comprises a cylinder body with a heat exchange jacket, wherein planar end closures are arranged at the upper and lower ends of the cylinder body, and a concentric inner cylinder body is arranged in the cylinder body; the upper end closure is provided with a mixed gas leading-out pipe; the lower end closure is provided with a three-way gas intake pipe; and a reaction solution eduction pipe and a feed liquid ingress pipe are arranged on the cylinder body. The process of preparing phosphorus pentafluoride comprises the following steps: blowing the reactor with an inert gas; creating a low temperature environment of the reactor with a refrigerant; adding a phosphorous pentachloride solution, anhydrous hydrogen fluoride and the inert gas to the reactor for reaction; and continuously leading out mixed gas containing phosphorus pentafluoride and part of a low-concentration phosphorous pentachloride solution, and at the same time continuously adding a phosphorous pentachloride concentrated solution, anhydrous hydrogen fluoride and the inert gas to realize continuous operation. The internal circulation reactor and method for continuously preparing phosphorus pentafluoride have the advantages that the concentration stability of reactants in the reactor can be maintained, and continuous production and automatic control of phosphorus pentafluoride are realized.

The invention discloses a synthesis method of 5-(4'-methyl-[1,1'-biphenyl]-2-yl)-1-hydro-tetrazole, which comprises the following steps: by using 2-carboxy-4'-methyl biphenyl as the raw material, reacting with excessive thionyl chloride under reflux conditions, depressurizing to remove excess thionyl chloride, and carrying out acylation reaction on benzsulfamide to obtain a product III; reacting the product III with phosphorous pentachloride by using carbon tetrachloride as a solvent to obtain an imino acyl chloride derivative IV; carrying out substitution reaction on the imino acyl chloride derivative IV and hydrazine hydrate to obtain a product V; and finally, carrying out cyclization on the product V and sodium nitrate under acidic conditions, and carrying out benzenesulfonyl removal reaction to obtain the 5-(4'-methyl-[1,1'-biphenyl]-2-yl)-1-hydro-tetrazole. The method has the advantages of mild reaction conditions, high safety and high efficiency.

The present disclosure provides an electrolyte composition and a metal ion battery comprising the same. The electrolyte composition comprises a metal halide; a solvent, wherein the solvent is a halogen-containing ionic liquid or an organic solvent, and the molar ratio of the metal halide to the solvent is 1:1 to 2.2:1; and, an additive , wherein the additive is added in an amount of 0.1-25wt%, based on the total weight of the metal halide and the solvent. The additive is monochloroethane, trichloroethylene, dichloroethane, trichloroethane, phosphorus trichloride, phosphorus pentachloride, picoline, methyl nicotinate, or a combination of the above. The electrolyte composition of the present invention can improve the conductivity of the electrolyte composition, increase the capacity of the metal ion battery, shorten the charging time, and prolong the cycle life of the metal ion battery.

The invention discloses a preparation process of high-purity phosphorus pentafluoride, which comprises the following steps of: firstly adding phosphorous pentachloride into a feed hopper of a spiral feeder under the protection of dry gas in a glove box to assemble a gas circulation loop, and simultaneously adding inert gas into the gas circulation loop in advance; starting a spiral stirring reaction furnace, simultaneously injecting mixed gas of hydrogen fluoride and fluorine gas into the spiral stirring reaction furnace, and controlling the reaction process by controlling the rotation frequency of the phosphorous pentachloride in the spiral feeder, the temperature of gas flow at the outlet of the spiral stirring reaction furnace and the pressure of the gas circulation loop; freezing the phosphorus pentafluoride gas and the hydrogen fluoride gas generated in the reaction process and unreacted hydrogen fluoride gas by a condenser-evaporator, and collecting high-purity phosphorus pentafluoride gas after reaction. The method is simple and effective and can be operated easily.