92 results about "Diethylamine" patented technology

The invention relates to the technical field of chemical synthesis, and particularly discloses a compound with a peculiar smell removing function as well as a preparation method and application thereof. The chemical name of the compound is 2-ethoxy-3-((E)-methoxy-3-oxopropyl-1-alkene-1-yl) phenyl cinnamate, the smell of the compound is extremely light, sulfur-containing and nitrogen-containing compounds causing stink can be captured through a Michael addition reaction, and efficient peculiar smell removal is achieved. The preparation method comprises the following steps: (1) taking cinnamic acid as an initial raw material, and reacting with diethylamino sulfur trifluoride to prepare cinnamic acid acyl fluoride; (2) carrying out an esterification reaction on the cinnamic acid acyl fluoride and 2-methoxy-3-hydroxybenzaldehyde in the presence of 4-dimethylaminopyridine, so as to obtain 2-methoxy-3-formyl phenyl cinnamate; and (3) carrying out Wittig reaction on the 2-methoxy-3-formyl phenyl cinnamate and a phosphorus ylide reagent, so as to obtain the target compound.

This invention provides an ethyl-containing alkoxy-terminated organosilicon polymer, its preparation method, and its applications. The preparation method includes: S1, mixing methylvinylcyclotetrasiloxane, a solvent, and a first catalyst, introducing hydrogen gas, and reacting at 50-70°C until the methylvinylcyclotetrasiloxane content is no higher than 5%, filtering to remove impurities and obtain the product; S2, under nitrogen protection, ring-opening the product obtained in step S1 with acetic anhydride in the presence of a ring-opening catalyst, neutralizing and hydrolyzing, removing impurities, and obtaining the product; S3, under nitrogen protection, reacting the product of step S2 with hexamethyldisilazane at 40-50°C for 1-3 hours, adding N,N-diethylamino-trialkoxysilane, and reacting at 50-60°C for 1-3 hours. The polymer obtained by this invention, as a thermally conductive powder treatment agent, can effectively improve the dispersion performance of powders and enhance the heat resistance of products without reducing their tensile strength.

The application relates to the technical field of wastewater treatment, and discloses an expanded graphite catalyst for degrading chemical pharmaceutical wastewater and a preparation method. In the application, 2,2'-diamino-N-(hydroxypropyl trimethyl ammonium chloride) diethylamine is used to carry out an amidation reaction with carboxyl groups on the surface of oxidized expanded graphite, so as to bond and introduce active functional groups such as amino groups, quaternary ammonium salts and hydroxyl groups on the surface of the expanded graphite; then, through high-temperature hydrothermal reaction, zinc oxide particles are uniformly generated in the expanded graphite, and the expanded graphite catalyst is obtained. The active groups such as the hydroxyl groups of the expanded graphite catalyst form hydrogen bonds and other interactions with tetracycline hydrochloride, so that the adsorption and removal rate of the tetracycline hydrochloride is improved. The zinc oxide particles are uniformly grown in the expanded graphite matrix and are not prone to agglomeration, and a large number of photocatalytic active sites are exposed, so that the expanded graphite catalyst has better photocatalytic degradation performance on the tetracycline hydrochloride.

The invention relates to the technical field of wastewater treatment, and discloses an expanded graphite catalyst for degrading chemical pharmaceutical wastewater and a preparation method of the expanded graphite catalyst. 2, 2 '-diamido-N-(hydroxypropyl trimethyl ammonium chloride) diethylamine and carboxyl on the surface of oxidized expanded graphite are subjected to an amidation reaction, and the expanded graphite catalyst is prepared. Active functional groups such as amino, quaternary ammonium salt and hydroxyl are bonded and introduced to the surface of the expanded graphite, then zinc oxide particles are uniformly generated in the expanded graphite through a high-temperature hydrothermal reaction, and the expanded graphite catalyst is obtained. Active groups such as hydroxyl of the expanded graphite catalyst and tetracycline hydrochloride form hydrogen bonds and interact with each other, so that the adsorption and removal rate of tetracycline hydrochloride is increased. Zinc oxide particles uniformly grow in an expanded graphite matrix, are not easy to agglomerate, expose a large number of photocatalytic active sites, and have better photocatalytic degradation performance on tetracycline hydrochloride.

The invention discloses a preparation method of a bilastine intermediate, which comprises the following steps: reacting a compound 5 with thionyl chloride under the conditions that dichloromethane is used as a solvent and DMF (Dimethyl Formamide) is used as a catalyst to generate acyl chloride, and then reacting the acyl chloride with diethylamine to prepare a compound 6; taking dichloromethane as a solvent, and carrying out Friedel-Crafts acylation on the compound 6 and ethyl oxalyl chloride under the condition of anhydrous aluminum trichloride to obtain a compound 7; reducing the compound 7 by using sodium borohydride, liquid caustic soda and a water system to prepare a compound 8; taking dichloromethane as a solvent, and reducing the compound 8 by TMDS under the condition of anhydrous aluminum trichloride to prepare a compound 9; hydrolyzing the compound 9 under the hydrochloric acid condition to obtain a compound 10; and under the condition of thionyl chloride, carrying out esterification reaction on the compound 10 and methanol to prepare the bilastine intermediate TM. The preparation method of the bilastine intermediate, provided by the invention, has the advantages of economical and easily available raw materials, mild reaction conditions, efficient reaction and simple operation, and is suitable for industrial application.

The present application belongs to the technical field of pharmaceutical therapy, and particularly relates to an amide-substituted tryptophan ketone derivative, a preparation method and application thereof. The structural formula of the tryptophan ketone derivative is shown in formula (A) or formula (B). In the formula, n=1 or 2, and R is any one of dimethylamine group, diethylamine group, morpholine group, 1-methylpiperazine group, cyclopropylamine group and 4-hydroxypiperidyl group. The compound can selectively inhibit the activity of acetylcholinesterase, and has the potential to develop into a drug for treating Alzheimer's disease due to the abilities of self-aggregation and the like. 1‑42 ​

The invention discloses an aluminum-based catalyst for producing triethylamine through reaction of coal-based ethanol and diethylamine. The active component is loaded on the carrier; the rod-like morphology is fully utilized, the dispersity of active metal can be effectively improved, the isolation effect of Sn is achieved, after hydrogen reduction, oxidation-state cobalt becomes reduction-state cobalt more easily, distribution of the reduction-state cobalt in rod-like aluminum oxide is more uniform, agglomeration is not prone to occurring in the reaction process, and the reaction efficiency is improved. The diffusion of reactants and products in the catalyst and the improvement of the reaction activity of the catalyst are facilitated; when the catalyst is used for producing triethylamine through reaction of coal-based ethanol and diethylamine, compared with a CoSn / Al2O3 (irregular morphology) catalyst, the selectivity of triethylamine can be obviously improved. The active components are elemental cobalt and elemental tin.

The invention relates to the field of monoethylamine preparation processes, and discloses a monoethylamine production method, which comprises: under the action of an ammonolysis catalyst, uniformly mixing and preheating diethylamine, hydrogen and ammonia gas, allowing diethylamine to pass through an ammonolysis reactor and a deamination tower, carrying out monoethylamine refining, diethylamine refining and triethylamine refining, and preparing monoethylamine, the ammonolysis catalyst comprises a carrier as well as an active component and an auxiliary agent which are loaded on the carrier, and is characterized in that the carrier is aluminum oxide modified by a titanium silicalite molecular sieve, the content of the aluminum oxide exceeds 68wt% of the total mass of the carrier, the active component comprises nickel, the auxiliary agent comprises iridium, and the content of the titanium silicalite molecular sieve is more than 68wt% of the total mass of the carrier. On the basis of the total weight of the ammonolysis catalyst, the content of the nickel element is 15-30 wt%, and the content of the iridium element is 0.2-2 wt%. By adopting the method disclosed by the invention, monoethylamine can be directly produced by taking diethylamine as a raw material.

The application designs a method for preparing optically active methyl fluoropropionate by using diethylamine sulfur trifluoride, comprising the following steps: fluorination reaction: under the protection of nitrogen, methyl S-lactate is added to a dry reaction kettle as raw material, the kettle temperature is cooled to a first reaction temperature, diethylamine sulfur trifluoride is added dropwise into the reaction kettle, after dropping, the reaction kettle is heated to a second reaction temperature, after the reaction is completed, the reaction mixture is added dropwise into saturated sodium / potassium bicarbonate aqueous solution to obtain R-2-fluoropropionic acid methyl ester; the molar ratio of diethylamine sulfur trifluoride to methyl S-lactate is 1-1.5:1, the method is high in efficiency, low in three-waste amount, short in reaction path, suitable for industrial production, and has economic value.

This invention belongs to the field of chemical catalyst preparation technology, and discloses a catalyst for the disproportionation of diethylamine to triethylamine. The catalyst includes a support, and MgO, ZnO, and rare earth oxides supported on the support. The content of each component, based on 100% mass, is as follows: support 80-85%, MgO 5-10%, ZnO 5-10%, and rare earth metal oxides 2-5%. When used for the disproportionation of diethylamine to triethylamine, the catalyst exhibits high diethylamine conversion and high selectivity for the triethylamine product. After separation, unreacted diethylamine can be recycled, while monoethylamine is collected separately or recycled back to the diethylamine synthesis unit, significantly reducing overall costs.

The invention relates to the technical field of production of monoethylamine and acetonitrile by using ethylenediamine and refining and separation thereof, and discloses a method for co-production of monoethylamine and acetonitrile, which comprises the following steps: (S1) in the presence of a catalyst, diethylamine, hydrogen and ammonia gas are uniformly mixed and preheated, and then are subjected to an ammonolysis reactor reaction and gas-liquid separation, and a crude product obtained after gas-liquid separation passes through a monoethylamine refining tower to obtain a monoethylamine product; separating into a monoethylamine product at the top of the tower and a tower kettle product containing diethylamine and acetonitrile at the bottom of the tower; the catalyst comprises aluminum oxide modified by an SAPO-34 molecular sieve, Ni, Co, Pr and / or Nd, the content of Ni and Co is 15-40 wt%, and the molar ratio of Ni to Co is 1-8.5; (S2) separating a tower kettle product containing diethylamine and acetonitrile, which is led out by the monoethylamine refining tower, into a solvent-containing material flow at the tower top and an acetonitrile product at the tower kettle through an acetonitrile refining tower; according to the method, monoethylamine and acetonitrile products are produced at the same time through diethylamine ammonolysis reaction and rectification separation.

The application relates to a water-based ink with high adhesion and a preparation process thereof, wherein the water-based ink at least comprises the following raw materials in mass parts: 100-140 parts of acrylic emulsion; 120-160 parts of titanium white powder; 20-60 parts of ethylene glycol; 0-5 parts of functional additives; 80-100 parts of organic pigment; 400-600 parts of deionized water; porous cellulose, the added mass of the porous cellulose is 0.08-0.16 times the sum of the mass of the acrylic emulsion and the titanium white powder, and the Zeta potential of the porous cellulose at pH=7 is not more than -45 mV; the porous cellulose is obtained by dissolving cellulose diacetate, solidifying and phase separating, and then hydrolyzing and regenerating in a hydrolysis bath, the hydrolysis bath is an aqueous solution of sodium hydroxide and a potential adjusting agent, and the potential adjusting agent is at least one of triethylamine, diethylamine and ammonia water. The water-based ink in the application not only has good adhesion with a printing substrate, but also has good adhesion in itself.

The invention discloses a preparation process of electronic-grade bis (diethylamino) silane, and relates to the technical field of chemical synthesis. The preparation process of the electronic-grade bis (diethylamino) silane at least comprises the following preparation steps: dehydrating monosilane through a low-temperature adsorption tower to obtain dehydrated monosilane, and separating heavy components from diethylamine through a molecular sieve membrane to obtain purified diethylamine; reacting the dehydrated monosilane with the purified diethylamine in the presence of a palladium-loaded catalyst to obtain crude bis (diethylamino) silane; and carrying out reduced pressure rectification on the crude bis (diethylamino) silane to separate low-boiling-point substances, and carrying out complexing adsorption on the low-boiling-point substances by using an ethylenediamine tetraacetic acid modified silica gel bed layer to remove metal ions so as to obtain the electronic-grade bis (diethylamino) silane. The purity of the prepared electronic-grade bis (diethylamino) silane is greater than or equal to 99.9995%, the chloride ion content is less than or equal to 20ppb, the total amount of metal impurities is less than or equal to 8ppb, the reaction yield is greater than or equal to 91%, and the comprehensive energy consumption is reduced by more than 50%.

The invention discloses an HPLC (High Performance Liquid Chromatography) detection method for ipragmine hydrochloride enantiomers, and belongs to the technical field of pharmaceutical analysis. The HPLC detection method provided by the invention comprises the following steps: dissolving ipragmine hydrochloride to be detected in a diluent to prepare a test solution; detecting the test solution by adopting normal-phase high performance liquid chromatography; the stationary phase of the normal-phase high performance liquid chromatography is silica gel of which the surface is covalently bonded with cellulose-tri (3-chloro-4-methyl phenyl carbamate); a mobile phase of the normal-phase high performance liquid chromatography is a mixed solution of normal hexane, isopropanol, trifluoroacetic acid and diethylamine. According to the detection method established by the invention, the ipragmine hydrochloride main peak and the S-configuration enantiomer impurity peak can be subjected to baseline separation, the separation degree can reach 4.5 or above, the method is high in specificity and sensitivity, and various methodology verification parameters all meet the drug quality control requirements.

The invention provides a crystal form of a compound HIF-117 salt as well as a preparation method and application of the crystal form, and the crystal form is any one or more of the following crystal forms: a hydrochloride crystal form A, a sulfate crystal form B, a 1, 2-ethanedisulfonate crystal form C1, 1, 2-ethanedisulfonate crystal form C2, 1, 2-ethanedisulfonate crystal form C3 and 1, 2-ethanedisulfonate crystal form C4. The crystal form 1, 2-ethanedisulfonate crystal form C2, p-toluenesulfonate crystal form D, mesylate crystal form E1, mesylate crystal form E2, hydrobromide crystal form F1, hydrobromide crystal form F2, sodium salt crystal form G, sylvite crystal form H1, sylvite crystal form H2, calcium salt crystal form I, magnesium salt crystal form J, choline salt crystal form K, lysine salt crystal form L, ammonium salt crystal form M, meglumine salt crystal form N, betaine salt crystal form O1, betaine salt crystal form O2 and diethylamine salt crystal form P1, the invention relates to a diethylamine salt crystal form P1, a diethylamine salt crystal form P2, a diethylamine salt crystal form P3, a diethylamine salt crystal form P4, a diethylamine salt crystal form P5, a tromethamine salt crystal form Q1, a tromethamine salt crystal form Q2 and a tromethamine salt crystal form Q3. The compound has good stability, and has important value for development and production of medicines and preparations.

The invention discloses a method for detecting cyclohexyl isocyanate in a gliquidone raw material medicine. Diethylamine is adopted for derivation, cyclohexyl isocyanate and diethylamine are subjected to a derivation reaction, and the residual quantity of the impurity cyclohexyl isocyanate in the gliquidone raw material medicine is detected through a liquid chromatography-mass spectrometry method. The method has high system applicability, has incomparable advantages in specificity, quantitation limit, detection limit, linear range and repeatability, and has high precision.

The invention discloses a treatment method of a florfenicol by-product N, N-diethyl-2, 3, 3, 3-tetrafluoropropionamide, and belongs to the technical field of chemical engineering, the treatment method comprises a hydrolysis addition reaction and a cyclization reaction; the hydrolysis addition reaction comprises the following steps: mixing N, N-diethyl-2, 3, 3, 3-tetrafluoropropionamide with diethylamine and alkali liquor, and then carrying out hydrolysis reaction and addition reaction to obtain N, N, N ', N'-tetraethyl malonamide; the cyclization reaction comprises the following steps: mixing organic solvent solutions of N, N, N ', N'-tetraethyl malonamide and sodium methoxide, adding a mixed solution of formamidine and an organic solvent, carrying out reflux heat preservation reaction, evaporating materials to dryness, acidifying and filtering. According to the method, the malonamide intermediate is generated through fewer reaction steps, then the 4, 6-dihydroxypyrimidine is prepared, most of materials can be recycled, the atom economy is high, and the pollution to the environment and the post-treatment pressure are also reduced.

The invention discloses a production device and a production method of diethylamine, which adopt a cyclic operation process of raw material preheating, reaction, multi-extraction sequential rectification, by-product transalkylation, pressurized gradient condensation, reduced pressure cooling heat exchange and low-temperature hydrogen recovery, and acetonitrile is hydrogenated to generate a hydrogenated product containing diethylamine. The method has the advantages that the raw material conversion rate and the diethylamine process yield are effectively increased, unreacted hydrogen can be recycled, the raw material conversion rate is further increased, and the method is convenient to operate, low in cost and suitable for industrial production. The method is suitable for industrial large-scale production; the production device and the production method can be used for continuous cycle production of industrial diethylamine, are convenient to operate, are suitable for industrial large-scale production, and can effectively improve the conversion rate of raw materials and the yield of diethylamine, and meanwhile, the process can recycle related intermediate products, has fewer by-products, and is greener and more environmentally friendly.

The invention discloses a method for synthesizing a camptothecin chiral precursor with high enantioselectivity, and belongs to the field of organic synthesis. In the invention, the preparation of a chiral precursor amide compound of camptothecin comprises the following steps: synthesizing corresponding aryl (E)-2-ethylbutyl-2-olefine acid ester, mixing the aryl (E)-2-ethylbutyl-2-olefine acid ester with a phase transfer catalyst derived from cinchona alkaloid in an organic solvent, sequentially adding acid, potassium permanganate and a small amount of potassium fluoride solution for reaction, and after the reaction is finished, performing suction filtration to obtain the chiral precursor amide compound of camptothecin. Carrying out amine ester exchange with diethylamine; and evaporating the solvent, and quickly purifying by using a silica gel column to obtain the camptothecin precursor chiral amide compound with high enantioselectivity. The invention aims at providing a new thought and a new method for total synthesis of camptothecin based on a camptothecin chiral precursor reported in literatures, and broadens a synthesis route for synthesizing camptothecin.

The invention discloses a near-infrared two-region imaging material and a preparation method and application thereof, and belongs to the technical field of photoelectric functional materials. The near-infrared two-region imaging material is an aza-fluorine boron pyrrole derivative NJ1040; the preparation method comprises the following steps: dissolving 2-acetylthiophene in ethanol to obtain a mixed solution, adding a potassium hydroxide aqueous solution, stirring, adding 4-diethylaminobenzaldehyde, stirring, and extracting; drying the extracted organic phase, and performing rotary evaporation concentration and purification to obtain an intermediate I; mixing the intermediate I, diethylamine and nitromethane, reacting, extracting, drying the extracted organic phase, and performing rotary evaporation concentration and purification to obtain an intermediate II; mixing the intermediate II, ammonium acetate and ethanol for reaction, adding triethylamine and a boron trifluoride diethyl etherate complex for continuous reaction after rotary evaporation concentration, and extracting; and drying the extracted organic phase, carrying out rotary evaporation concentration, and purifying to obtain the product. NJ1040 nanoparticles are prepared by a nano coating technology, so that the problem of poor solubility of a contrast agent is solved.

The utility model discloses a tetraethylthiuram disulfide production reaction device which comprises a reaction kettle, a stirring structure is arranged in the reaction kettle, a jacket is arranged outside the reaction kettle, and an ethanol solution adding pipeline, a diethylamine adding pipeline, a hydrogen peroxide adding pipeline and a carbon disulfide adding pipeline are arranged at the top end of the reaction kettle. The ethanol solution adding pipeline is connected with a liquid outlet of the ethanol solution static mixer, an ethanol inlet pipeline and a soft water inlet pipeline are arranged on the ethanol solution static mixer, and the carbon disulfide gas discharging pipeline is connected with a gas inlet of the condenser; a condensate outlet pipeline of the condenser is connected with a carbon disulfide receiving tank, a bottom outlet pipeline of the carbon disulfide receiving tank is connected with a carbon disulfide adding pipeline, the carbon disulfide adding pipeline is further connected with a carbon disulfide transfer pump, and a carbon disulfide metering pump is arranged on the carbon disulfide adding pipeline. One-step safe production of tetraethylthiuram disulfide can be realized, and the production efficiency is improved.

The invention discloses a high performance liquid chromatography (HPLC) detection method for enantiomers in moxifloxacin hydrochloride with high separation degree, and belongs to the technical field of medicine detection. The method aims at solving the problems that in the prior art, the leading edge of a main component peak is serious, and the detection accuracy and good peak pattern under the conditions of high separation degree and low content are difficult to meet at the same time, and the adoption of an expensive chiral chromatographic column is avoided. According to the detection method, chiral resolution is realized on a conventional high performance liquid chromatograph by adopting a reversed-phase chromatographic column (such as terminated octadecylsilane chemically bonded silica as a filler). According to the core technical scheme, the unique mobile phase composition is as follows: a water phase contains 0.54 g / L of zinc acetate and 1.17 g / L of L-valine, 1ml of diethylamine is creatively added, and the pH value is adjusted to 5.6 by using dilute sulfuric acid; and an organic phase adopts a methanol-ethanol mixed solution (15: 8) with a specific ratio. And finally, mixing the water phase and the organic phase according to the volume ratio of 77: 23. Under optimal chromatographic conditions (the column temperature is 40 DEG C and the detection wavelength is 295 nm), the method can realize efficient separation between moxifloxacin hydrochloride and enantiomers, the separation degree is greater than 4.5, and the detection accuracy of trace isomers can be realized. A methodological verification result shows that the method is high in sensitivity (the detection limit is 0.0096%, and the quantitation limit is 0.024%), and has a good linear relationship (a correlation coefficient rgt; and the accuracy is good (the recovery rate is between 80.0% and 120.0%). The method can be used for qualitative and quantitative analysis of the moxifloxacin hydrochloride bulk drug and enantiomers in the moxifloxacin hydrochloride preparation.

The invention discloses a method for preparing tetraethylthiuram disulfide through combined catalysis of a metal catalyst and solid alkali, and belongs to the technical field of organic synthesis. The method comprises the following steps: filling a continuous flow fixed bed with molybdenum disulfide and calcium hydroxide to form a composite multi-catalyst, preparing a reaction raw material solution from carbon disulfide and diethylamine as raw materials, controlling the flow of the reaction raw material solution and the flow of gas entering a reactor, and carrying out a temperature-controlled and pressure-controlled reaction to obtain a reaction solution; and carrying out post-treatment on the reaction liquid to obtain tetraethylthiuram disulfide. Molybdenum disulfide and calcium hydroxide are adopted to form a composite multi-term catalyst, a heterogeneous catalysis reaction is accurately controlled, the tetraethylthiuram disulfide crystal is obtained only through crystallization, filtration and drying of a prepared crude product, the purity and yield of the obtained tetraethylthiuram disulfide are high, and the method is environmentally friendly, high in atom economy and suitable for industrial production. Conditions are mild, the catalyst can be recycled, and products are easy to separate.

The invention provides a preparation method of diethylaminoethanethiol, which comprises the following step: enabling gaseous episulfide ethane and gaseous diethylamine to be in contact for reaction to obtain reaction liquid containing diethylaminoethanethiol. The preparation method of the diethylaminoethanethiol provided by the invention is simple and convenient to operate, and the diethylaminoethanethiol can be obtained with high yield and high purity.

The application discloses SAPO-18-MeR molecular sieve and a preparation method and application thereof. The anhydrous chemical composition of the molecular sieve is mMe*nR(Si x Al y P z )O2; Me is at least one selected from Li + , Na + , K + and NH4 + ; R is at least one selected from N, N-diisopropyl ethylamine, tetraethyl ammonium hydroxide, triethylamine, diisopropylamine, diethylamine and ethylenediamine; m is the mole number of Me, m=0.05-0.2; n is the mole number of R, n=0.05-0.2; x is the mole fraction of Si, x=0.05-0.35; y is the mole fraction of Al, y=0.35-0.55; z is the mole fraction of P, z=0.25-0.45, and x+y+z=1. The molecular sieve has excellent silicon distribution and strong acid property, and has excellent catalytic performance as a denitration catalyst after loading Cu ions.

The invention discloses a preparation method of a plant growth regulator maleic acid bis (diethylamino) ethanol ester citrate compound, which comprises the following steps: placing maleic anhydride and diethylamino ethanol in a container containing a stirring device, a reflux condensation device and a temperature control device according to a specific molar ratio, and heating under the protection of inert gas to carry out acylation reaction; after acylation is completed, adjusting the temperature, and adding citric acid to carry out salt forming reaction; after salt formation is finished, primarily separating by a separating device, and removing impurities by refining equipment to obtain a refined solution; and then controlling crystallization conditions to crystallize and separate out the product, and finally obtaining the final product through a specific drying mode. In the preparation process, parameters such as material ratio, temperature, time, stirring speed and the like in each reaction stage as well as separation, crystallization and drying conditions are accurately set, so that the maleic acid bis (diethylamino) ethanol ester citrate compound with high purity and high quality can be stably prepared.

The invention belongs to the field of chemical analysis, and particularly discloses a method for determining diethylamine based on derivatization reaction-HPLC (high performance liquid chromatography) and application thereof, and the method comprises the following steps: adding excessive 1-naphthyl isocyanate into a diethylamine solution, carrying out nucleophilic addition reaction to generate an ultraviolet absorption derivative 1-naphthyl diethylurea, and carrying out column chromatography on the 1-naphthyl diethylurea to obtain 1-naphthyl diethylurea; the method comprises the following steps: determining the peak area of 1-naphthyl diethylurea by adopting a high performance liquid chromatography, drawing a calibration curve by taking the mass concentration of diethylamine as a horizontal coordinate and the peak area of 1-naphthyl diethylurea as a vertical coordinate, and realizing quantitative determination of diethylamine based on the calibration curve, the molar ratio of the 1-naphthyl isocyanate to the diethylamine is 5: 1. Specific recognition of derivatization reaction is realized by utilizing the chemical structure difference between diethylamine (secondary amine) and triethylamine (tertiary amine), triethylamine cannot react with 1-naphthyl isocyanate, matrix interference is thoroughly eliminated in cooperation with physical separation of HPLC gradient elution, and the content of diethylamine can be specifically recognized and measured.

The application discloses a synthesis method of azanirmite raw medicine, and relates to the technical field of medicine synthesis. The synthesis method of the azanirmite raw medicine comprises the following synthesis steps: S1, a nucleophilic substitution reaction of 2,6-dichloropyridazine and mercaptoacetic acid is carried out to obtain 2-((6-chloropyridazine-3-yl)thio)acetic acid; and S2, an amide condensation reaction of 2-((6-chloropyridazine-3-yl)thio)acetic acid and diethylamine is carried out to obtain azanirmite. The azanirmite raw medicine can be synthesized through two-step reactions, and has the advantages of easy-to-obtain raw materials, mild reaction conditions, simple operation, high product yield and high purity, and is suitable for industrialized production of the azanirmite raw medicine.

The invention discloses a method for detecting N-nitrosodiethylamine in diclofenac epolamine, which comprises the following steps: dissolving a diclofenac epolamine sample in a methanol solution, adding a formic acid aqueous solution, mixing, and precipitating out diclofenac epolamine in the sample; centrifugally separating, and taking supernate; and carrying out quantitative detection on the N-nitrosodiethylamine in the supernate by adopting a liquid chromatography-tandem mass spectrometry method. Based on the principle that diclofenac is converted into free acid to be precipitated under the acidic condition, 2% formic acid is creatively selected as a precipitator, matrix interference of main components is effectively removed, the problem that the main components are separated out in a chromatographic system is solved, and a mass spectrometer is protected. According to methodology verification, the method disclosed by the invention is extremely high in sensitivity, good in accuracy, strong in reproducibility, rapid in analysis and good in durability. The method provides a reliable and efficient detection means for quality control of trace N-nitrosodiethylamine in the diclofenac epolamine bulk drug, and has extremely high practical value.