35 results about "Methylamine hydrochloride" patented technology

The invention belongs to the technical field of lithium ion batteries, and discloses a carbon compatible binder for a silicon-carbon negative electrode of a lithium ion battery and a preparation method and application of the carbon compatible binder for the silicon-carbon negative electrode of the lithium ion battery. Then N-hydroxysuccinimide and 1-ethyl-(3-dimethylaminopropyl) carbodiimide are added to activate carboxyl of sodium carboxymethyl cellulose, finally 1-pyrene methylamine hydrochloride is added, N2 is introduced at the room temperature, and a reaction is performed under stirring. According to the binding agent, sodium carboxymethyl cellulose is used as a main chain to be subjected to amidation reaction with 1-pyrene methylamine hydrochloride, pi-pi conjugation can be formed by introduced pyrene groups and graphite in a silicon-carbon material, the interface compatibility of the binding agent and the silicon-carbon material can be effectively improved, the dispersity and the binding property of the silicon-carbon material are enhanced, and the binding agent can be used for preparing the silicon-carbon material. And the electrochemical performance of the silicon-carbon negative electrode of the lithium ion battery is obviously improved.

The invention relates to a method for optimizing the quality of a perovskite layer through atmosphere annealing, and belongs to the technical field of perovskite layer quality optimization, and the method comprises the steps: preparing precursor materials: taking methylamine hydrochloride, cesium iodide, formamidine iodide and lead iodide as perovskite precursor materials; the preparation method comprises the following steps: preparing a solvent: mixing N-methyl pyrrolidone with dimethylformamide; solution preparation: mixing the precursor material with a solvent to prepare a precursor solution; stirring and filtering the solution; preparing a substrate: sputtering NiO serving as a hole transport layer material on the glass substrate; blade coating of a perovskite precursor solution: uniformly blade coating the precursor solution on the glass substrate coated with the NiO film; preliminary drying; vacuum annealing preparation: placing the glass substrate coated with the perovskite precursor film in a vacuum cavity; nitrogen atmosphere filling: filling high-purity nitrogen; in the nitrogen atmosphere, the temperature in the cavity is increased to a certain temperature range, annealing is conducted at the temperature, and the optimized annealing temperature and time are selected; and cooling and packaging.

The invention discloses a preparation method of deuterated methylamine hydrochloride and a solid-phase continuous flow synthesis system, and relates to the technical field of deuterated synthesis. The preparation method comprises the following steps: adding out-of-phase polykadexide into methyl trifluoromethanesulfonate and 1, 2-dichloroethane for heating reaction, then adding methanol for quenching reaction, washing and drying to obtain an out-of-phase polykadexide type methyl reagent; the method comprises the following steps: adding a heterophase polysulfide-type methyl reagent into a mixed solvent of a polar solvent and heavy water, and carrying out alkali treatment to complete deuteration conversion, so as to obtain a heterophase polysulfide-type deuterated methyl reagent; the preparation method comprises the following steps: dissolving o-phenylsuccinimide in acetonitrile, and adding a heterophase polysulfide deuterium methyl reagent and inorganic alkali to react, so as to obtain N-(1, 1, 1-trideuterium methyl) benzo-succinimide; the preparation method comprises the following steps: hydrolyzing N-(1, 1, 1-trideuterium methyl) benzo-succinimide and hydrochloric acid in an aqueous solvent to obtain deuterated methylamine hydrochloride. The preparation method is simple, the deuterium source is cheap, the atom utilization rate is high, the deuteration rate is high, and the production cost is low.

The invention belongs to the technical field of laminated photovoltaic cells, and particularly provides a preparation method of a wide-band-gap perovskite solar cell, which is used for solving the problems that in the prior art, a wide-band-gap perovskite light absorption layer has too many defects and is poor in phase separation and crystallization quality, so that carrier transmission is hindered, and the service life of the wide-band-gap perovskite solar cell is prolonged. And the open-circuit voltage and the efficiency of the perovskite solar cell are reduced. Methylamine hydrochloride (MACL) and phenethyl ammonium acetate (PEAAc) are introduced as precursor additives in the preparation process of the perovskite light absorption layer, the MACL can significantly inhibit degradation of a perovskite precursor solution, and the preparation of a high-quality perovskite thin film with oriented growth and excellent crystallization is facilitated; nH2 of PEAAc can provide Pb < 2 + > electrons to passivate halogen vacancies; moreover, through the synergistic effect of the MACL and the PEAAc, a perovskite thin film with better crystallization quality and fewer defects can be obtained, so that the open-circuit voltage and the photoelectric conversion efficiency of a perovskite solar cell device are effectively improved.

The invention provides a preparation method of (5-fluoro-2, 3-dihydrobenzofuran-4-yl) methylamine hydrochloride, the (5-fluoro-2, 3-dihydrobenzofuran-4-yl) methylamine hydrochloride is a compound as shown in a formula a, and the preparation method comprises the following steps: adding a compound b into an acid solution to remove Boc protecting groups to obtain a compound a, and adding a compound b into a reaction kettle to obtain a compound b; according to the preparation method, an eight-step synthesis route is provided, the (5-fluoro-2, 3-dihydrobenzofuran-4-yl) methylamine hydrochloride is prepared through the eight-step reaction of formylation, deprotection, substitution, upper protection, ring closing, deprotection, ammonification and deprotection, dangerous equipment such as a highly toxic reagent, an expensive palladium catalyst and high-pressure hydrogenation is not used in the whole reaction process, and the preparation method is simple and convenient to operate and easy to implement. The yield of each step is higher than that of the prior art.

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 invention belongs to the technical field of organic synthesis, and particularly provides a preparation method of (trimethylsilyl) methylamine hydrochloride. The preparation method provided by the embodiment of the invention comprises the following steps: carrying out reduction reaction on N-[(trimethylsilyl) methyl] benzylamine, and salifying with hydrochloric acid to generate (trimethylsilyl) methylamine hydrochloride. According to the preparation method disclosed by the embodiment of the invention, milder reduction hydrogenation operation is selected, severe conditions such as high temperature and high pressure are avoided, and the reaction yield and the product purity are improved.

The invention provides a method for synthesizing N,3,3-trimethyl-2-oxobutyramide. 3,3-dimethyl-2-oxobutyric acid is used as a raw material, and methylamine hydrochloride is reacted with an organic base and a condensing agent to generate N,3,3-trimethyl-2-oxobutyramide. The yield of N,3,3-trimethyl-2-oxobutyramide generated by the synthesis method of the invention is high, the yield reaches 82%, the reaction conditions are mild, it is suitable for scaled-up production, and no highly toxic raw materials are used, which is safe and environmentally friendly.

The present application belongs to the technical field of laminated photovoltaic cell, and specifically provides a preparation method of a wide-bandgap perovskite solar cell, to solve the problem that in the prior art, the wide-bandgap perovskite light-absorbing layer has too many defects, phase separation and poor crystalline quality, which hinders the carrier transport, and further leads to the problem of low open-circuit voltage and low efficiency of the perovskite solar cell. 2+ In the preparation process of the perovskite light-absorbing layer, methylamine hydrochloride (MACL) and phenethylammonium acetate (PEAAc) are introduced as precursor additives, MACL can significantly inhibit the degradation of the perovskite precursor solution, and is conducive to the preparation of high-quality perovskite thin film with oriented growth and excellent crystalline quality; NH2 of PEAAc can provide Pb 2+ electrons, passivate halogen vacancies; and the synergistic effect of MACL and PEAAc can obtain perovskite thin film with better crystalline quality and fewer defects, thereby effectively improving the open-circuit voltage and photoelectric conversion efficiency of the perovskite solar cell device.

The invention provides atomoxetine hydrochloride and a preparation method thereof, and relates to the technical field of medicinal chemistry and organic synthesis. The method provided by the invention comprises the following steps: adopting acetophenone, methylamine hydrochloride and a formaldehyde aqueous solution as raw materials, carrying out Mannich reaction to construct a beta-amino carbonyl skeleton, reducing carbonyl into hydroxyl by adopting sodium borohydride, then reacting with di-tert-butyl dicarbonate to form an amino protecting group, adopting o-methylphenol as a raw material, and preparing the beta-amino carbonyl skeleton. The method comprises the following steps: adding p-toluenesulfonic acid monohydrate and a (2-hydroxybenzyl) phosphine oxide catalyst to construct an ether bond through a Mitsunobu reaction, then removing a t-butyloxycarboryl protecting group, and carrying out chiral resolution and salinization reaction by using S-mandelic acid to obtain atomoxetine hydrochloride. The method of dropwise adding the formaldehyde aqueous solution in batches and controlling the reaction temperature is adopted, so that the generation of impurities can be reduced, and the yield is effectively improved; the p-toluenesulfonic acid monohydrate and the (2-hydroxybenzyl) phosphine oxide catalyst capable of participating in catalytic circulation are used for catalyzing the Mitsunobu reaction, the economic principle is met, and the purity and the yield of the product are greatly improved.

The invention relates to a perovskite precursor solution, a perovskite thin film, a preparation method of the perovskite thin film and a photovoltaic module. The perovskite precursor solution comprises a perovskite precursor, an additive and a mixed solvent; the perovskite precursor is prepared from formamidine hydriodate and lead iodide; the additive comprises cesium iodide and methylamine hydrochloride; the mixed solvent is prepared from N, N-dimethyl formamide, N-methyl pyrrolidone and cyclohexyl pyrrolidone. The composition of the perovskite precursor solution is blended, the high-quality perovskite thin film with the micro-suede surface is spontaneously formed in the perovskite crystallization process, the micro-suede surface structure can increase the contact area between a perovskite layer and a subsequent functional layer, a tight mechanical interlocking effect is generated between the micro-suede surface structure and the interface of the functional layer, and the performance of the perovskite thin film is improved. Therefore, the interface adhesive force of the subsequent functional layer and the metal electrode is obviously improved, and the problem of performance degradation of the perovskite assembly caused by the packaging process is solved.

The invention relates to the technical field of oil field clay stabilizers, in particular to a trihydroxy quaternary ammonium salt micromolecular clay stabilizer as well as a preparation method and application thereof, and the trihydroxy quaternary ammonium salt micromolecular clay stabilizer can be obtained by reacting methylamine hydrochloride and 2, 3-epoxypropyl trimethyl ammonium chloride serving as reaction raw materials at a certain temperature. The prepared trihydroxy quaternary ammonium salt micromolecular clay stabilizer is a trihydroxy quaternary ammonium salt aqueous solution, the trihydroxy quaternary ammonium salt contains strong polar molecules of four cations and three hydroxyls, the molecular weight is small, the charge density is high, the washing resistance is high, the clay expansion prevention effect is remarkable, and the temperature resistance reaches 207 DEG C; the preparation method is simple, safe and controllable in reaction process and suitable for large-scale production; the molecular weight is small, and secondary damage to the reservoir is avoided.

The invention relates to the technical field of pesticide synthesis, in particular to a method for synthesizing a saflufenacil intermediate, which comprises the following steps: taking ethyl trifluoroacetoacetate and 2-chloro-4-fluoro-5-aminobenzoate as raw materials, reacting under the action of alkali, and continuously evaporating out low-boiling-point alcohol in the reaction process to obtain an intermediate 1; then adding methylamine hydrochloride turbid liquid into the system, and performing azeotropic dehydration in the reaction process to obtain an intermediate 2; and finally, introducing a phosgene reagent into the system, and carrying out ring closing on the obtained intermediate 2 to obtain a target product. According to the method, cheap and easily available raw materials are used, a uracil ring is directly constructed through a one-pot three-step reaction, and the saflufenacil intermediate is synthesized, so that the process operation is greatly simplified; the target product synthesized by the method has higher yield and purity, the cost is reduced, the solvent can be recycled, the emission of three wastes is reduced, and the subsequent industrial production of saflufenacil is facilitated.

The invention belongs to the technical field of chemistry, and particularly relates to a preparation method of a glyoxylic acid derivative-13C. Comprising the following steps: carrying out nitrogen replacement on # imgabs0 # methylamine hydrochloride, a formaldehyde solution, K13CN and deionized water, adding NaOH after complete reaction, and heating to generate an intermediate substance 2-methylaminoacetic acid-1-13C; the method comprises the following steps: adding Br2 into a reaction kettle, stirring NaOH and deionized water, adding Br2, stirring at room temperature for 1 hour to obtain a reaction solution, dropwise adding a reaction system of 2-methylaminoacetic acid-1-13C into the obtained reaction solution, stirring until no 2-methylaminoacetic acid-1-13C exists, adjusting the pH value to 2-3, extracting, merging organic phases, washing, and performing chromatography to obtain the 2-glyoxylic acid-1-13C. The method has the advantages of easily available raw materials and high yield.

The invention provides a deuterated methylamine hydrochloride green synthesis method based on a continuous flow technology, which seamlessly integrates photocatalytic nitrification, catalytic hydrogenation and online acidification salification into a continuous and compact technological process through the continuous flow technology. And one-stop continuous synthesis from a gaseous raw material to a high-purity product is realized under a mild condition. Inert C-D bonds in deuterated methane can be efficiently activated at near room temperature in the core photocatalytic nitration step, and compared with a traditional high-temperature and high-pressure process, energy consumption is greatly reduced; the deuterated methane is used as a raw material, the use of a highly toxic reagent is avoided from the source, a continuous flow reaction system is combined with integrated water electrolysis for hydrogen production, the liquid holdup is small, and the intrinsic safety is high; meanwhile, a new way is provided for high-value utilization of deuterated methane, and the iron-based photocatalyst is low in cost and environmentally friendly and has good recycling potential.

The invention relates to a preparation method of sodium sarcosinate, which comprises the following steps: mixing a chloroacetic acid aqueous solution and a sodium carbonate aqueous solution to obtain a first mixed solution; feeding the first mixed solution into a methylamine aqueous solution for reaction to obtain a second mixed solution containing sodium sarcosinate, methylamine hydrochloride and methylamine; lye is fed into the second mixed solution for methylamine recovery, and tail gas containing methylamine and a third mixed solution with methylamine removed are obtained; and concentrating the third mixed solution to obtain a material containing sodium sarcosinate. The sodium sarcosine prepared by the method is high in purity, low in cost, good in fluidity and convenient to transport, store and use. In addition, the whole process of the preparation method provided by the invention basically does not generate solid waste and wastewater, so that waste is avoided, and the preparation method is green and environment-friendly.

The invention discloses a preparation method of N-demethylated ribociclib, which comprises the following steps: step 1, adding a solvent A into a compound (1), adding a condensing agent B, stirring to generate an intermediate state, continuously adding methylamine hydrochloride and triethylamine, and continuously carrying out acid amine condensation reaction to generate a compound (2); 2, dropwise adding a metal reagent solution D into a 4-(6-aminopyridine-3-yl) piperazine-1-carboxylic acid tert-butyl ester tetrahydrofuran solution under the protection of nitrogen, carrying out a heat preservation reaction after dropwise adding, adding a compound (2), and carrying out a heating reaction to generate a compound (3); and 3, removing Boc from the compound (3) in a solvent G under an acid E condition, concentrating and recovering the solvent, adjusting the pH value, and filtering to obtain a compound (4). The method has the advantages of cheap and easily available raw materials, simple steps, high yield and low total cost. The ribociclib succinate impurity reference substance prepared by the method is high in purity, can be used as a ribociclib succinate impurity reference substance, and has great significance in impurity research of the ribociclib succinate impurity reference substance. # imgabs0 #

The invention discloses a method for enhancing the stability of a perovskite film, which comprises the following steps of: 1, spin-coating a hole transport layer solution on a substrate, and heating to obtain a hole transport layer; 2, dissolving PbI2, deuterated formamidine iodide and methylamine hydrochloride in DMF and DMSO solvents, spin-coating the obtained hole transport layer with the solution, washing the hole transport layer with an anti-solvent before spin-coating is finished, placing the hole transport layer in air after spin-coating is finished, annealing for the first time, and then annealing for the second time to obtain a perovskite thin film; and step 3, cooling the perovskite thin film, spin-coating the electron transport layer material solution, continuously spin-coating the hole barrier layer solution, heating, cooling, and evaporating an electrode to obtain the perovskite solar cell. The deuterated formamidine iodide is used as a raw material to deposit the perovskite thin film, the photoelectric conversion efficiency of the prepared perovskite solar cell reaches 25.08%, and the original efficiency is maintained to be 97% or above after the perovskite solar cell is illuminated for 1264 hours.

The utility model belongs to the technical field of monomethylamine hydrochloride storage, and particularly discloses a monomethylamine hydrochloride storage device which comprises a storage box and a plurality of sealing paper tubes, a plurality of evenly-distributed storage bins are formed in the upper end face of the storage box, and the sealing paper tubes are located in the storage bins respectively. A movable plate located below the sealing paper tube is slidably connected into the storage bins, a fixed bin located below the multiple storage bins is arranged in the storage box, and the fixed bin communicates with the multiple storage bins through a plurality of groove holes correspondingly. Therefore, the sealing paper tube filled with monomethylamine hydrochloride is stored under the conditions of ventilation and drying and proper temperature, so that moisture accumulation and harmful gas accumulation are prevented, a low-temperature environment can be provided, the storage life of the sealing paper tube is prolonged, the stability of the sealing paper tube is kept, the sealing paper tube can be protected from being in contact with water, and the service life of the sealing paper tube is prolonged. And the sealing paper tube filled with the methylamine hydrochloride at the corresponding position can be conveniently taken out.

The invention discloses a multifunctional composite binder for a silicon-carbon negative electrode of a lithium ion battery as well as a preparation method and application of the multifunctional composite binder, and belongs to the technical field of lithium batteries. The method comprises the following steps: dissolving sodium alginate in a PBS buffer solution, adding a catalyst and 1-pyrene methylamine hydrochloride, carrying out an amidation reaction at room temperature, and carrying out precipitation, suction filtration and freeze-drying after the reaction is finished to obtain SA-Py; and adding water into the SA-Py to obtain an SA-Py aqueous solution, and dispersing the carboxylated carbon nanotubes in the SA-Py aqueous solution to obtain the multifunctional composite binder. The binder prepared by utilizing multiple synergistic effects effectively inhibits the volume expansion of the silicon-carbon negative electrode material in the cycle process, so that the long-term cycle stability of the electrode is remarkably improved.

The invention discloses a double-response small-molecule fluorescent probe for synchronously detecting NTR and nucleic acid and preparation and application thereof. A preparation method of the double-response small-molecule fluorescent probe comprises the following steps: adding 4-fluoro-3-methoxybenzaldehyde, potassium carbonate and methylamine hydrochloride into ethanol, and performing reflux reaction to obtain an intermediate NB1; the preparation method comprises the following steps: dissolving NB1, 4-methylpyridine and potassium tert-butoxide in N, N-dimethylformamide under the protection of nitrogen, and heating and stirring for reaction to obtain an intermediate NB2; the preparation method comprises the following steps: dissolving NB2, (4-nitrophenyl) methylsulfonyl chloride and triethylamine in dichloromethane under the protection of nitrogen, and reacting to obtain an intermediate NBP; the preparation method comprises the following steps: dissolving NBP, methyl iodide and triethylamine in dichloromethane under the protection of nitrogen, and stirring at room temperature until the reaction is completed to obtain a target product, namely the double-response small-molecule fluorescent probe. The NTR activity and the nucleic acid state in the biological sample can be synchronously and visually detected, and a more reliable technical scheme is provided for precise tumor detection and mechanism research.

The invention discloses a synthesis process of 6-hydroxytropinone, and relates to the technical field of chemical synthesis. When the 6-hydroxytropinone is prepared, diatomite, aluminum trichloride, zirconium sulfate tetrahydrate and octyltriethoxysilane are subjected to a reaction, and hydrophobic solid acid is prepared; the method comprises the following steps of: electrolyzing furan and ammonium bromide to prepare 2, 5-dimethoxy dihydrofuran, and reacting the 2, 5-dimethoxy dihydrofuran with hydrophobic solid acid to obtain 2-hydroxy-1, 4-butanedialdehyde; the preparation method comprises the following steps: preparing acetone dicarboxylic acid, methylamine hydrochloride and sodium acetate into a buffer solution, reacting 2-hydroxy-1, 4-butanedialdehyde with the buffer solution, and purifying and drying to obtain the 6-hydroxytropinone. According to the synthesis process of the 6-hydroxytropinone, the production time is shortened, the yield is increased, and the synthesis process is more economical and environment-friendly.

A method for synthesizing a stable isotope-labeled toltrazuril-D3 belongs to the field of organic synthesis technology. This method uses methylamine hydrochloride-D3 as the stable isotope labeling source, reacting it with p-trifluoromethylthiophenol and 1-chloro-2-methyl-5-nitrobenzene as starting materials, undergoing sequential condensation and reduction to obtain an aminodiphenyl ether intermediate. Simultaneously, methylamine hydrochloride-D3 reacts with sodium cyanate to generate methylurea-D3, which then reacts with carbonyl diimidazole to obtain an activated intermediate. Finally, the aminodiphenyl ether intermediate condenses with the activated intermediate, followed by base-catalyzed cyclization to obtain the target product, toltrazuril-D3. This invention features a rationally designed synthetic route, readily available raw materials, mild reaction conditions, simple operation, and easy product separation and purification. The obtained product achieves a chemical purity and isotope abundance of over 99%.

The application provides a preparation method of a palladium-tin-gallium ternary alloy nanomaterial, which comprises the following steps: A) under the protection of inert gas, mixing a metal palladium precursor, a metal tin precursor, a metal gallium precursor, methylamine hydrochloride, tri-octyl phosphine and oleylamine, and performing a warming reaction to obtain a preliminary reaction solution; and B) further performing a warming reaction on the reaction solution, washing and drying the reaction solution to obtain the palladium-tin-gallium ternary alloy nanomaterial. The preparation method is simple in operation and controllable in reaction conditions, and the obtained nanomaterial is spherical in shape, uniform in size and good in dispersity. The component of the nanomaterial can be accurately controlled by adjusting the feeding ratio of the metal precursors. The carbon-loaded nanomaterial catalyst prepared by loading the nanomaterial on a carbon carrier has excellent catalytic activity and stability for the electrocatalytic oxidation reaction of various alcohols, and has important application prospects in the field of new energy technologies such as direct alcohol fuel cells.

The invention provides a pyrrole sulfonic acid compound salt form as well as a preparation method and application thereof, and relates to 1-(5-(2-fluorophenyl)-1-3-(3-methoxypropoxy) benzenesulfonyl)-1H-pyrrole-3-yl)-N-methylamine organic acid salt which is prepared by the following steps: suspending pamoxamic acid and water, heating and stirring, slowly adding inorganic alkali, and keeping heating until the solution is clear; the preparation method comprises the following steps: slowly dropwise adding an aqueous solution of 1-(5-(2-fluorophenyl)-1-3-(3-methoxypropoxy) benzenesulfonyl)-1H-pyrrole-3-yl)-N-methylamine hydrochloride, heating, and carrying out a stirring reaction to obtain a reaction solution containing a target product; and cooling to precipitate a crude product of the target product from the reaction liquid, filtering, washing and drying to obtain the target product. By developing the low-solubility salt form, the effect of changing the water solubility of the medicine can be achieved, so that the release time of the patent medicine is effectively controlled, and the clinical medication requirement of continuous acid inhibition is met.

The utility model relates to the technical field of monomethylamine hydrochloride production and processing, in particular to monomethylamine hydrochloride drying equipment which comprises a drying tank, a mounting shaft is arranged in the drying tank, the outer wall of the mounting shaft is fixedly connected with a plurality of dispersing plates which are distributed up and down and are of a conical structure, monomethylamine hydrochloride is dispersed through the vibrating dispersing plates in a vibrating mode, and the monomethylamine hydrochloride is dried. According to the monomethylamine hydrochloride dispersing device, monomethylamine hydrochloride evenly falls into the uppermost material receiving groove, then the monomethylamine hydrochloride is gathered through the vibrating material receiving groove, moves towards the material passing opening and falls onto the next dispersing plate through the material passing opening, and in the falling process of the monomethylamine hydrochloride, the monomethylamine hydrochloride is evenly heated and dried through hot air. According to the monomethylamine hydrochloride drying device, the monomethylamine hydrochloride can be rapidly dried through multiple times of dispersion and convergence of the monomethylamine hydrochloride, then the dried monomethylamine hydrochloride is discharged out of the drying tank through the discharging port, and then the monomethylamine hydrochloride is continuously dried, so that the monomethylamine hydrochloride drying efficiency is improved.

The invention discloses a preparation method of 1-aminocyclohexyl methylamine hydrochloride. The preparation method comprises the following steps: S1, cyclohexanone, a cyaniding reagent and ammonia water react to produce 1-aminocyclohexyl cyanide; and S2, reducing the 1-aminocyclohexyl cyanide, and salifying to prepare the 1-aminocyclohexyl methylamine hydrochloride. The method has the advantages that the reaction conditions are mild, strict control of anhydrous conditions is not needed, additional catalysts are not needed, the 1-aminocyclohexyl cyanide can be obtained by the Strerecker reaction with high yield under the mild reaction conditions, and the average yield is 90% or above. The obtained 1-aminocyclohexyl cyanide is reduced by lithium aluminum hydride, so that the 1-aminocyclohexyl methylamine hydrochloride can be obtained at high yield.

The invention discloses a preparation method of deuterocoxitinib, and belongs to the technical field of chemical synthesis. According to the scheme, 4, 6-dichloropyridazine-3-carboxylic acid methyl ester is used as an initial raw material, and a target product is efficiently synthesized through four-step reaction of nucleophilic substitution, ammonolysis / hydrolysis, amide condensation and targeted condensation. A noble metal catalyst is not needed, a key carbon-nitrogen bond is constructed through a high-selectivity nucleophilic substitution process, deuterated methylamine hydrochloride is accurately introduced in a final step, and the reaction stability and selectivity are improved; the process is mild in condition and simple and convenient to operate, the final product yield exceeds 85%, the product purity reaches 99.8% or above, the used solvent and reagent are environment-friendly, free of heavy metal residues, few in waste liquid and waste residue and easy to treat, the green chemistry concept is completely met, and an efficient, economical and safe industrial path is provided for large-scale production of deuterocoxitinib.

The invention relates to a preparation method of a paroxetine main intermediate as shown in a formula I (-)-trans-4-(4-fluorophenyl)-3-hydroxymethyl-1-methylpiperidine. The preparation method comprises the following steps: by taking methyl p-fluorobenzoylacetate as a raw material, carrying out asymmetric hydrogenation to obtain an intermediate shown in a formula II; reacting the intermediate shown in the formula II with sodium methoxide and methylamine hydrochloride to obtain an intermediate shown in a formula III; generating an intermediate IV from the intermediate III under the action of reducing agents such as lithium aluminum hydride; reacting the intermediate shown in the formula IV with malonic acid monoester at room temperature to obtain an amide intermediate shown in the formula V; reacting the intermediate formula V with various chlorophosphodiesters at room temperature to obtain an intermediate formula VI; generating an intermediate formula VII from the intermediate formula VI under an alkaline condition; the intermediate formula VII generates a formula I (-)-trans-4-(4-fluorophenyl)-3-hydroxymethyl-1-methylpiperidine under the action of reducing agents such as lithium aluminum hydride. The process has the characteristics of relatively high yield, simple process, environmental friendliness and the like, and has a relatively good industrial application prospect. # imgabs0 #

The present invention relates to the field of organic synthesis technology, and more particularly to an electrochemical synthesis method for quinazolinone derivatives. In the present invention, an isatoic anhydride compound, a styrene compound, a methylamine hydrochloride compound, an electrolyte, and an organic solvent are mixed to obtain a reaction solution. The reaction solution is then energized to induce an electrochemical reaction, thereby obtaining the quinazolinone derivative. This method does not require the use of metal catalysts or strong oxidants, and reaction media such as the electrolyte and solvent are recyclable. It has the advantages of readily available raw materials, simple operation, and environmental friendliness.