30 results about "Dimethylamine hydrochloride" patented technology

The invention relates to a method for green, mild and efficient synthesis of methylamine hydrochloride based on photocatalysis. According to the method, methanol and ammonium chloride which are wide in source and low in price are used as raw materials, under the anaerobic condition, a Pd / TiO2 photocatalyst is adopted for a photocatalytic reaction, and target methylamine hydrochloride products including monomethylamine hydrochloride, dimethylamine hydrochloride and trimethylamine hydrochloride are synthesized in one step. Compared with traditional industrial synthesis, the photocatalysis technology has the advantages of mild reaction conditions, simplicity and convenience in operation, environmental friendliness and the like, provides an efficient and feasible way for green synthesis of methylamine hydrochloride, and has a wide application prospect.

The application provides an organic-inorganic hybrid zirconium-based polyacid derivative, which has a molecular formula of [H2N(CH3)2]4[Zr(DL-tartH)2(SbW 10 H8[Zr(DL-tartH)2(SbW 17 )2]·36H2O. 58 The zirconium-based polyacid derivative is prepared by mixing DL-tartaric acid, sodium tungstate, dimethylamine hydrochloride, Na9[SbW9O 33 ]·19.5H2O and ZrOCl2·8H2O in water in a certain proportion and reacting under water bath conditions. The application explores the photochromic process under the irradiation of a 300W xenon lamp, the discoloration process after the photochromic process under the conditions of room temperature, 50±5 DEG C and 80±5 DEG C respectively, and the discoloration process of the photochromic process under different oxygen concentrations. It is found that the mechanism of the photochromic process is mainly caused by W 6+ →W 5+ charge transfer, and the zirconium-based polyacid derivative can be used as a photochromic material, especially a reversible photochromic material. The target product 1 is dissolved in distilled water and coated on cellulose filter paper, and the xenon lamp coloring can show obvious blue color, realizing inkless printing.

The present disclosure provides a preparation method for metformin hydrochloride. The preparation method includes: microwave heating raw materials containing dicyandiamide and dimethylamine hydrochloride, and reacting the two at 100° C. to 160° C. to obtain a product system containing metformin hydrochloride. Microwave heating is adopted to heat the dicyandiamide and the dimethylamine hydrochloride. Compared with a conventional heating mode that requires heat to be gradually transferred from the outside to the inside, microwave heating can directly heat each part inside the reactant, which can make the internal temperature of the reactant more uniform, thereby reducing the generation of impurities.

The invention belongs to the technical field of catalysts, and provides a novel polyacid catalyst of which the molecular formula is [(CH3) 2NH2] 9 [SbIII3 (A-alpha-PW9O34) 2]. 7H2O. The polyacid catalyst is prepared by mixing and dissolving sodium dihydrogen phosphate, dimethylamine hydrochloride and Na9 [SbW9O33]. 19.5 H2O according to a certain proportion in water and reacting under a water bath condition. Under the reaction conditions of normal temperature, normal pressure and no solvent, the application of the catalyst to synthesis of diaryl methane and derivatives thereof by green catalysis of aldehyde and indole reaction is studied.

The application belongs to the technical field of organic synthesis, and specifically discloses a preparation method of dimethyl diallyl ammonium chloride, which comprises the following steps: under the condition that water exists, dimethylamine, an alkaline carrier and allyl chloride are mixed and subjected to a contact reaction to obtain a crude tertiary amine; the alkaline carrier comprises a carrier body and a carbonic acid alkali metal salt loaded on the carrier body; under the condition that an organic solvent exists, the crude tertiary amine and allyl chloride are mixed and subjected to a contact reaction. The method can effectively reduce the hydrolysis of allyl chloride and the generation of dimethylamine hydrochloride in the reaction process, the dimethyl diallyl ammonium chloride product contains almost no other hydrochloride impurities, and the reaction efficiency, the yield and the purity of the dimethyl diallyl ammonium chloride are improved.

The present invention provides a uranium-containing tellurium tungstate, a preparation method and an application thereof, belonging to the technical field of new polyacid chemistry materials. The chemical formula of the present invention is [H2N(CH3)2] 14 Na4[(UO2)2(H2O)2(Te3W 21 O 75 H)2]·18H2O, belonging to the monoclinic system, space group P21 / n, and the unit cell parameters are: #imgabs0# α = γ = 90°, β = 89.899°, #imgabs1# Z = 4. After stirring sodium tungstate, sodium perchlorate and sodium tellurite in an aqueous solution, dimethylamine hydrochloride is added and the pH is adjusted, and then uranyl nitrate is added for a water bath reaction followed by post-treatment to obtain the uranium-containing tellurium tungstate. The uranium-containing tellurium tungstate of the present invention has a clear structure and good stability, and has photochromism. Its preparation process is simple and easy to operate.

The present invention relates to an organic germanium ligand and samarium ion-functionalized antimony tungstate material with the chemical formula: Na4[H2N(CH3)2] 16 H 18 [Sm4(H2O) 12 W4O 14 Ge(CH2CH2COOH)]2[SbW9O 33 4[Ge(CH2CH2COOH)SbW 15 O 54 2·56H2O. The synthesis of this material uses an organic germanium ligand and an Sb 3+ ion double-template induced synthesis strategy, and is prepared by a one-step self-assembly reaction using antimony trichloride solution, sodium tungstate, di(carboxyethyl)germanium sesquioxide, dimethylamine hydrochloride and samarium nitrate. This preparation method is simple and easy to implement, and has a low cost. In addition, the organic germanium ligand and samarium ion-functionalized antimony tungstate material are compounded with gold nanoparticles to obtain a nanocomposite material with good stability and high photothermal conversion efficiency. The application of this composite material in the photothermal therapy of breast tumor cells shows good therapeutic effects, indicating that the organic ligand and rare earth-functionalized antimony tungstate material have certain application potential in tumor treatment, tumor drugs, photothermal therapy and other aspects.

This invention relates to a dimethylamine-modified tetranuclear heterometallic cluster compound, its preparation method, and its application. The invention is intended for the field of electrocatalytic oxygen evolution and relates to a compound, its preparation method, and its application. The purpose of this invention is to address the problem of hydrogen energy shortage. The dimethylamine-modified tetranuclear heterometallic cluster compound has the molecular formula [(CH3)2NH2][Ni(H2O)6][{NaNiSbW(OH)4(H2O)6}{SbW8O 30 Na₂[SbW₁₉O]·2H₂O has a molecular weight of 2861.62. It is used for alkaline electrocatalytic oxygen production. Preparation method: Prepare Na₂[SbW₁₉O]₂. 33 Precursor; Na9[SbW9O 33 The precursor was dissolved in deionized water, nickel nitrate was added, and the mixture was stirred. Terephthalic acid was added, and the mixture was stirred again. NaOH solution was added dropwise, and the reaction was allowed to proceed for 2 hours. After cooling, the mixture was filtered, and dimethylamine hydrochloride was added. The mixture was then evaporated at room temperature to crystallize. Hexagonal yellow crystals appeared after three days, yielding the product. The overpotential of the dimethylamine-modified tetranuclear heterometallic cluster compound of this invention can reach 39.7 mV. The Tafel slope is 19.75 mV / dec. The slope of the fitted straight line is 4.51 mF / cm. 2 Electrochemical transfer resistance: 1.9Ω.

The invention discloses a method for detecting dimethylamine in levofloxacin, which comprises the following steps: weighing levofloxacin, adding a diluent for dissolving and diluting, and taking filtrate to obtain a test solution; taking a dimethylamine hydrochloride reference substance, and adding a diluent for dissolving and diluting to obtain a reference substance solution; respectively injecting the reference solution and the test solution into an ion chromatograph, recording chromatograms, and calculating by peak areas according to an external standard method to obtain the content of dimethylamine. According to the method for detecting the dimethylamine in the levofloxacin, the content of the dimethylamine in the levofloxacin is measured through the ion chromatography, the method is simple, convenient and feasible, high in specificity, high in accuracy and good in repeatability, the method has the advantages of being high in detection sensitivity, the content of the dimethylamine in the levofloxacin raw material can be accurately and sensitively detected, and the detection cost is low. Therefore, the quality of the levofloxacin raw material is ensured.

The utility model relates to the technical field of wastewater treatment, and particularly discloses a low-concentration DMF (Dimethyl Formamide) wastewater treatment device which comprises a lifting pump, a heat exchanger, an alkali adding device, a mixer, an alkaline hydrolysis tank, a gaseous membrane component, an absorption liquid storage tank, an absorption liquid circulating pump, an evaporated liquid circulating pump, a forced circulation evaporator, a separator and an MVR (Mechanical Vapor Recompression) compressor, a gaseous membrane is adopted to absorb dimethylamine generated by alkaline hydrolysis, mass transfer power is the partial pressure difference of dimethylamine gas on the two sides of the membrane, dimethylamine is transferred from the interior of membrane filaments to the exterior of the membrane filaments to be absorbed by absorption liquid and reacts with the absorption liquid to generate dimethylamine salt, and therefore the high partial pressure is always kept on the wastewater side, and the partial pressure of dimethylamine on the absorption liquid side is extremely low; the whole process is large in mass transfer power and high in removal rate, dimethylamine hydrochloride in the absorption liquid is high in concentration and small in evaporation capacity, a large amount of energy consumption is saved compared with direct rectification, DMF in the wastewater can be converted into valuable dimethylamine hydrochloride through a series of chemical reactions, and crystals can be recycled after centrifugal separation and purification.

The invention relates to the technical field of chemical preparation, in particular to a preparation method of a reducing agent material dimethylamino borane for pretreatment of horizontal chemical copper deposition in a PCB (printed circuit board) process. The preparation method comprises the following steps: firstly adding an organic solvent I in an inert gas atmosphere, cooling to 0 DEG C or below, sequentially adding dimethylamine hydrochloride and sodium borohydride for reaction, and adding a mixed solvent for continuous reaction after the reaction is performed for a period of time; and separating and purifying the reaction product to obtain the product dimethylamino borane. The dimethylamino borane is prepared under the reaction condition of minus 10 DEG C to 0 DEG C, dimethylamine hydrochloride is firstly added into an organic solvent (such as tetrahydrofuran), then sodium borohydride is controlled to be added in batches, and nitrogen protection is carried out in a drying stage, so that by-products can be avoided, and the yield of the dimethylamino borane is effectively increased.

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a preparation method of tetramethylguanidine, which comprises the following steps: step 1, reacting cyanogen chloride with dimethylamine at low temperature in a tubular reactor to generate dimethylamino cyanogen and dimethylamine hydrochloride, step 2, heating intermediates of the dimethylamino cyanogen and the dimethylamine hydrochloride, and reacting to obtain the tetramethylguanidine. The method comprises the following steps: 1, adding a sodium hydroxide aqueous solution into a reaction solution, carrying out heat preservation on the reaction solution after adding a catalyst, and carrying out high-temperature condensation to generate tetramethylguanidine hydrochloride, 3, cooling the product, filtering to obtain tetramethylguanidine hydrochloride, and washing the tetramethylguanidine hydrochloride with a detergent, and 4, carrying out a neutralization reaction on the sodium hydroxide aqueous solution and tetramethylguanidine hydrochloride to obtain the tetramethylguanidine hydrochloride. And extracting the reaction solution by using an organic solvent, and fractionating to obtain free tetramethylguanidine. The catalyst is added in the reaction process, so that the temperature required by the reaction is reduced, the time required by the reaction is shortened, a continuous flow process is realized, and the productivity is remarkably improved.

The invention relates to the technical field of industrial synthesis of small organic molecules, in particular to an industrial synthesis method of DMAB. According to the method, dimethylamine hydrochloride and NaBH4 serve as raw materials, THF and water serve as solvents, DMAB is prepared through the steps of feeding, reacting, aftertreatment, purification and the like in the inert gas atmosphere, large-amount dehydration of an organic phase and deep dehydration of a high-concentration product are achieved through two times of drying, and the drying efficiency and the product stability are both considered; the process sequence of reduced pressure distillation and recrystallization is adopted, and after low-temperature concentration and preliminary impurity removal, deep purification is achieved through low-temperature recrystallization. According to the method, the temperature is strictly controlled in the whole process, the inert atmosphere is maintained, the safety risk and product degradation are reduced, the product yield is stabilized at 86-92%, the purity is consistent with that of commercially available analytically pure products, the process steps are simplified, parameters are controllable, the number of times of solution transfer is reduced, mother liquor can be recycled, and the method has a good industrial application prospect.

The invention relates to the technical field of preparation of PCB (Printed Circuit Board) electronic chemical materials, in particular to a preparation method of a reducing agent material dimethylamino borane for pretreatment of horizontal chemical copper deposition in a PCB process. The raw materials comprise dimethylamine hydrochloride, sodium borohydride, sodium hydroxide and a solvent. The preparation method comprises the following steps: adding a solvent into a flask, then adding dimethylamine hydrochloride, and keeping high-speed stirring; replacing air in the flask with nitrogen; adding sodium borohydride into the flask in batches; preparing a mixed solution, and cooling; adding the prepared mixed solution into the flask in batches for continuous reaction; adding a sodium hydroxide solution and filtering; drying the mother liquor and then filtering; evaporating the mother liquor to remove a solvent, and filtering; and drying in vacuum to evaporate out the solvent, and recrystallizing to obtain the high-purity dimethylamino borane.

The utility model relates to a sucralose neutralization mother liquor rectifying and recycling device which comprises a first rectifying assembly, a second rectifying assembly and a third rectifying assembly, the first rectifying assembly comprises a first rectifying tower, a first condenser communicated with the top of the first rectifying tower and a first return tank connected with the first condenser and the first rectifying tower; the parameters of the first rectifying tower are as follows: the number of tower plates is 18-30, the tower top temperature is 20-40 DEG C, the tower bottom temperature is 80-100 DEG C, and the pressure in the tower is 8-15 bar; the byproduct utilization assembly comprises an ammonia distributor connected with the first reflux tank and a reactor communicated with the bottom of the first rectifying tower. The first rectification assembly with a specific structure is matched with the byproduct utilization assembly, so that ammonia water and dimethylamine hydrochloride with a specific concentration are obtained, the recycling of specific byproducts is realized, and the production profit is improved.

The present invention discloses a 1,4-dicarbonyl compound, its preparation method and application. The 1,4-dicarbonyl compound has the structure shown in Formula I. The preparation method includes the following steps: S1. Compound a reacts with thionyl chloride and dimethylamine hydrochloride to form compound b; S2. Compound b reacts with iodine, magnesium chips and 4-bromo-1-butene to form compound c; S3. Compound c reacts with dimethyl sulfide to obtain the compound with the structure shown in Formula I. Among them, the preparation method of the 1,4-dicarbonyl compound of the present invention is simple in operation and relatively mild in reaction conditions, and has broad application prospects.

The invention belongs to the technical field of fine chemical engineering, and particularly relates to a method for synthesizing 1, 1, 3, 3-tetramethylguanidine, which comprises the following steps: step 1, adding dimethylamine into a reaction flask, starting stirring, then controlling the temperature at 20-50 DEG C, introducing chlorine gas into the reaction liquid while adding hydrocyanic acid for 1-4 hours, reacting to generate dimethylamino nitrile and dimethylamine hydrochloride, and then adding the dimethylamine hydrochloride into the reaction flask to obtain dimethylamine hydrochloride; the method comprises the following steps: 1, preparing a reaction solution, 2, heating the reaction solution to carry out a condensation reaction so as to generate tetramethylguanidine hydrochloride, and 3, adding liquid caustic soda into the reaction solution to carry out alkalization so as to generate tetramethylguanidine, and sequentially carrying out dimethylamine recovery, solvent extraction, solvent concentration and rectification on the reaction solution so as to finally obtain tetramethylguanidine. The method is simple in technological process, mild in reaction condition, free of high-temperature and high-pressure operation, low in production risk and beneficial to large-scale production.

The present application relates to the technical field of flux processing. More specifically, it relates to a high-wetting halogen-free flux and a preparation method thereof. The high-wetting halogen-free flux is prepared from the following raw materials by weight percentage: film-forming agent 20-30%, active agent 4-8%, palm wax 5-10%, corrosion inhibitor 0.5-1%, thixotropic agent 2-5%, dimethylamine hydrochloride 0.2-0.6%, rare earth chloride 1-2%, modifier 5-10%, and the remaining amount is solvent. The modifier is obtained by mixing castor oil, stearic acid amide and glycerol. The halogen-free flux prepared by the above compounding formula greatly improves the wettability during the welding process, makes the molten pool more stable, and reduces the occurrence of welding defects. At the same time, the introduction of the modifier, especially the mixture of castor oil, stearic acid amide and glycerol, not only improves the thermal stability of the flux, but also reduces the risk of decomposition of traditional active agents at high temperatures, reduces the release of harmful gases and the formation of residues, and ensures the welding quality.

The invention relates to the technical field of tin wire welding of photovoltaic junction boxes, and discloses a special tin wire for a photovoltaic junction box and a manufacturing process of the special tin wire. The alloy layer comprises tin, lead, aluminum, antimony, arsenic, bismuth, copper, iron, zinc, cadmium and sulfur; the soldering flux layer is composed of rosin, tetrahydrofurfuryl alcohol, propylene glycol monomethyl ether, succinic acid, glutaric acid, dibromo butylene glycol, dimethylamine hydrochloride and a fluorocarbon surfactant; the softening agent is added into the raw materials in the soldering flux layer, the viscosity of the soldering flux layer is increased, the tin wire composed of the soldering flux layer and the alloy layer can be well attached to a welding spot after welding, residues of the tin wire after welding are transparent, the tin wire is not brittle, not prone to powdering and not sticky, the problem that production lines and products are polluted by rosin after welding is solved, meanwhile, the activity of the tin wire is excellent, and the service life of the tin wire is prolonged. According to the tin wire, the different proportions of the softening agent in the soldering flux layer are changed, so that the manufactured tin wire can be suitable for different temperature conditions.

The invention discloses an additive-containing mixed acid group all-vanadium redox flow battery positive electrode electrolyte and application thereof, and belongs to the technical field of redox flow battery energy storage. The positive electrode electrolyte comprises an additive and an active substance, wherein the additive is selected from one or two or more of dimethylamine hydrochloride, diethylamine hydrochloride, dipropylamine, butanediamine and nitrilotriacetic acid; the active substances are VO < 2 + > and VO < 2 + >. The preparation method comprises the following steps: step 1, firstly dissolving vanadyl sulfate in hydrochloric acid to obtain a hydrochloric acid solution of vanadyl sulfate, and then obtaining an electrolyte in an electrolysis mode; and 2, adding the additive into the electrolyte in the step 1, and stirring at room temperature until the additive is completely dissolved. When the positive electrode electrolyte is applied to the mixed acid-based all-vanadium redox flow battery, the problem of chlorine gas precipitation in the charging process of the battery can be obviously improved, the stability of the positive electrode electrolyte is improved, the battery performance of the battery in the long-term cycle process is effectively improved, and long-term stable operation of the battery is realized.

The application discloses a preparation method of fosnetupitant and intermediates thereof, which comprises the following steps: taking an amino thiophene compound II-a as a starting material, generating a chlorinated compound II-d through a plurality of reactions such as urea formation, ring closure and chlorination, then selectively catalytically hydrogenating and removing the chlorine at the C-4 position of the pyrimidine ring to obtain a compound II-e, and then preparing an intermediate compound II through ester hydrolysis and condensation with dimethylamine hydrochloride; taking a compound III-a and a compound III-b as starting materials to generate a substitution reaction to obtain a compound III-c, and then reducing the compound III-c through catalytic hydrogenation to obtain an intermediate compound III; and further generating a Buchwald-Hartwig coupling reaction of the intermediate compound II and the intermediate compound III to obtain a finished product of fosnetupitant. The preparation method can not only reduce the cost, simplify the synthesis route, control each reaction and improve the total yield, but also is more economic and environmental. Meanwhile, the application improves the stability and reliability of the process, and provides a guarantee for industrialized scale production of fosnetupitant.

The application belongs to the technical field of herbicides, and provides a preparation method of the herbicide cycloxaprid, which comprises the following steps: 1, mixing and stirring monocyanamide and ethyl chloroformate, cooling to 0-2 DEG C, adding liquid alkali dropwise, controlling pH and temperature, and carrying out incubation reaction to obtain a product GH520-1; 2, adding dimethyl sulfate and benzyl triethylammonium chloride to the product GH520-1, carrying out warming reaction, and after the reaction is completed, standing and layering to obtain a product GH520-2; 3, adding dimethylamine hydrochloride and liquid alkali to the product GH520-2, supplementing toluene, carrying out warming reaction, cooling to room temperature, standing and layering to obtain a product GH520-3; 4, dissolving the product GH520-3 in toluene, adding cyclohexyl isocyanate, and controlling the reaction temperature to obtain a product GH520-4; and 5, adding sodium methoxide and dimethylamine aqueous solution to the product GH520-4, controlling the reaction temperature, and obtaining a product GH520.

The invention relates to the technical field of preparation of dimethylamino borane, in particular to a method for preparing dimethylamino borane, which at least comprises the following steps: adding a mixed solvent into a reaction container in a nitrogen environment, cooling to 0-20 DEG C, adding dimethylamine hydrochloride, stirring and mixing; uniformly dividing sodium borohydride into 15-30 batches, adding one batch of sodium borohydride into the reaction container every 10-45 minutes, controlling the temperature rise not to exceed 3 DEG C, and continuously reacting for 0.5-2 hours after half of the total batch number is added; the method comprises the following steps: mixing a mixed solvent with water to obtain a solvent mixed solution, dividing the solvent mixed solution into 5-15 batches and the rest 5-15 batches of sodium borohydride, alternately adding the solvent mixed solution and the rest 5-15 batches of sodium borohydride into a reaction container, controlling the temperature to rise not to exceed 3 DEG C, reacting for 0.5-2 hours after the solvent mixed solution and the sodium borohydride are completely added, and then reducing the temperature of a reaction system to-10-0 DEG C, the product is obtained through further treatment, and the product purity and yield are guaranteed.

The invention relates to the technical field of tin alloy welding flux and welding materials, and discloses a high-corrosion-resistance tin wire. Scaling powder is arranged on the outer side of a tin wire body; the tin wire main body comprises tin and copper; the tin wire main body comprises the following components in parts by weight: 99.3 parts of tin; 0.7 part of copper; the soldering flux is composed of esterified rosin, tetrahydrofurfuryl alcohol, succinic acid, glutaric acid, dibromo butylene glycol and dimethylamine hydrochloride. The soldering flux comprises the following components in percentage by weight: 89-92% of esterified rosin; 4.5% to 5.5% of tetrahydrofurfuryl alcohol; 0.5%-1% of succinic acid; 0.5%-1% of glutaric acid; 1%-1.5% of dibromo butylene glycol; 1.4%-1.7% of dimethylamine hydrochloride; the soldering flux added on the tin wire main body is improved, and the esterified rosin with low corrosivity is selected as a carrier, so that the corrosivity of the whole soldering flux is reduced, meanwhile, the high activity of the soldering flux is ensured, and the situation that after the tin wire main body is welded, the corrosivity of residual soldering flux components on a mother part becomes strong, and consequently a welding part is bad and aged in advance is prevented.

The invention belongs to the technical field of industrial wastewater treatment and recycling, and discloses a method for treating washing wastewater in the production process of 2-chloro-5-chloromethylpyridine, which comprises the following steps: adding acid into the wastewater, adjusting the pH value of the system to 2.0-3.5, adding an oxidant and a catalyst for reaction, and decomposing dimethylamine hydrochloride; adding an organic phase composed of an extraction agent and a diluent into the pretreated wastewater, carrying out multi-stage counter-current extraction under the conditions that the temperature is 10-40 DEG C and the pH value is 1.5-3.0, and carrying out phase splitting to obtain a phosphoric acid-loaded organic phase and raffinate; carrying out back extraction on the organic phase loaded with phosphoric acid by using deionized water to obtain a phosphoric acid aqueous solution; carrying out reduced pressure distillation on the raffinate, and condensing and recovering the evaporated DMF and water vapor to obtain a DMF aqueous solution; residual liquid obtained by reduced pressure distillation passes through an adsorption column filled with an adsorbent. According to the method, the process contradiction between alkaline recovery of dimethylamine and acidic extraction of phosphoric acid is successfully solved, and efficient recovery and deep purification of high-value resources in the wastewater are realized.

The application provides a synthesis method of relugolix, comprising the following steps: reacting compound 2 with di-tert-butyl dicarbonate to obtain compound 3; reacting compound 3 with dibromohydantoin to obtain compound 4; reacting compound 4 with dimethylamine hydrochloride to obtain compound 5; hydrolyzing compound 5 to obtain compound 6; condensing compound 6 with 6-methoxy-3-aminopyridazine to obtain compound 7; deprotecting the amino group of compound 7 to obtain compound 8; performing reductive amination on compound 8 with 2,6-difluorobenzaldehyde to obtain compound 9; performing nitro reduction on compound 9 to obtain compound 10; and reacting compound 10 in the presence of carbonyldiimidazole and methoxyamine hydrochloride to obtain relugolix. The synthesis method is more efficient than prior art, avoids potential genotoxic impurities in the prior art, has mild process conditions, high reaction yield in each step, effectively reduces industrial production cost and safety risk, and is suitable for industrial production.

This invention relates to the field of wastewater treatment technology, and more particularly to a method and application for preparing dimethylamine hydrochloride from ODPA production wastewater. The method specifically includes the following steps: ODPA production wastewater is fed into a distillation column and distilled under vacuum with increased temperature; the gas then enters a condenser; under illumination, the non-condensable gas is washed with an alkaline solution containing a catalyst, and then the gas is absorbed using hydrochloric acid absorbent to obtain an aqueous solution of dimethylamine hydrochloride. This method can effectively separate N,N-dimethylformamide and dimethylamine from ODPA production wastewater. After washing the dimethylamine with an alkaline solution and absorbing it with hydrochloric acid, the resulting dimethylamine hydrochloride can be used as an organic byproduct in the production of aminoethyl sulfide, thus realizing the resource utilization of dimethylamine hydrochloride.

The invention provides a synthesis method for constructing chiral Ugi amine, and belongs to the technical field of organic synthesis. The method comprises the following steps: by taking ferrocene, an aldehyde compound and dimethylamine hydrochloride as initial raw materials, firstly, in a reaction system, generating an imine onium ion intermediate from the aldehyde compound and the dimethylamine hydrochloride in situ; then, under the action of a chiral supramolecular catalyst, ferrocene performs enantioselective nucleophilic addition on carbon of imidoonium ions, so that a chiral carbon center is efficiently constructed in one step, and chiral Ugi amine with high optical purity is obtained. According to the invention, a'one-pot method 'enantioselectivity construction strategy is adopted, an additional splitting or configuration inversion step is not needed, and the reaction efficiency and the optical purity can be remarkably improved. According to the method, the yield of the chiral Ugi amine is 90-99%, the enantiomer purity (ee value) is as high as 95-99%, a tedious enantiomer resolution or configuration inversion step in a traditional method is avoided, and the reaction efficiency and the atom economy are remarkably improved.

The invention discloses a high performance liquid chromatography method for detecting dimethylamino hydrochloride residues in dimethylaminochloroethane hydrochloride, and relates to the technical field of pharmaceutical analysis, acetonitrile is used as a solvent, a benzoyl chloride acetonitrile solution is used as a derivatization reagent, a sodium hydroxide solution is used as an acid-binding agent, dimethylamine hydrochloride and N, N-dimethylformamide are used as an acid-binding agent, and a high performance liquid chromatography method for detecting the dimethylamino hydrochloride residues in dimethylaminochloroethane hydrochloride is provided. The method comprises the following steps: reacting N, N-dimethylethanolamine hydrochloride with a benzoyl chloride acetonitrile solution under a heating condition; according to the method, the residues of dimethylamine hydrochloride and N, N-dimethylethanolamine hydrochloride in dimethylaminochloroethane hydrochloride can be effectively detected, the limit of quantitation reaches 0.4 mu g / ml of dimethylamine hydrochloride, and compared with an existing gas-phase and liquid-phase direct sample injection method, the used reagents and consumables are conventional consumables, so that the operation is safe and simple, the treatment is convenient and rapid, and the method is suitable for industrial production. The detection efficiency is improved, and the cost is reduced; equipment is easy to obtain, and a measured chromatographic baseline is stable and does not drift.