15 results about "Dimethylamine hydrochloride" patented technology

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.

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 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 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 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 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 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 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.