50 results about "Methylamine hydrochloride" patented technology

The invention provides a preparation method for preparing high-purity 5-(2-fluorophenyl)-N-methyl-1-(3-pyridine sulfonyl)-1H-pyrrole-3-methylamine fumarate. The method comprises the following steps: taking 5-(2-fluorophenyl)-N-methyl-1-(3-pyridine sulfonyl)-1H-pyrrole-3-methylamine hydrochloride as an intermediate; carrying out alkali treatment, and then salifying the treated intermediate with fumaric acid to obtain a finished product. A final product prepared by adopting the method has high purity and low content of key impurities; in addition, the purification and post treatment steps of fumarate are simplified, and the yield is remarkably improved.

The invention discloses a preparation method of naftifine hydrochloride, which uses N-methyl-1-naphthyl methylamine hydrochloride as raw material, to directly participate reaction without alkalization free purification, uses organic ether solvent as reaction solvent, in the presence of alkali metal carbonate and catalyst, at suitable temperature, to generate crude naftifine hydrochloride via condensation reaction, and feeds acetic ester saturated solution of hydrochloride to generate hydrochlorate, and obtains high-purity naftifine hydrochloride product via recrystallization. The invention completes alkalization free purification, and condensation reaction in one device, with simple operation, high yield, low foreign material content, low cost, and industrialization support, which is better than previous synthesis method.

The invention relates to a preparation method of Terbinafine hydrochloride, which comprises the following steps: dissolving a certain amount of catalyst, i.e. sodium iodide (or potassium iodide) in an organic solvent, adding 1-chloro-6,6-dimethyl-2-heptylene-4-alkyne, sequentially adding alkali and N-methyl-1-naphthalene methylamine hydrochloride, carrying out condensation at 10-40 DEG C, salifying the obtained product in an alcohol system with hydrogen chloride to obtain the Terbinafine hydrochloride, and carrying out recrystallization in an alcohol/water mixed solution to obtain the qualified product. In the method, the raw materials are cheap and easily-acquired, the reaction is complete, and the reaction time is greatly shortened. Therefore, the method is completely suitable for industrialized mass production.

The invention discloses a preparation method of N,O-dimethyl-N'-nitroisourea. According to the preparation method, O-methyl-N-nitroisourea and methylamine hydrochloride are used as a raw material, and water is used as a solvent, so that reaction is performed in a potassium fluoride-water system, wherein the chemical reaction formula is as shown in the specification. The preparation method disclosed by the invention is simple and convenient in process and simple in operation; the water is used as the solvent, the pH value is not needed to be regulated and a catalyst is not needed to be added, so that the generation of secondary reactions can be effectively inhibited. The purity of products can reach more than 99%, and the yield can reach 79.1%; the preparation method is suitable for industrial production.

The invention discloses a preparation for preventing and controlling bee fungal diseases. The preparation consists of 0.1 to 2 percent of (E)-N-(6,6-dimethyl heptanoic-2-olefin-4-alkynyl)-N-methyl-1-naphthalene methylamine hydrochloride, 0.1 to 4 percent of beneficial microorganism and 94 to 99.8 percent of soluble starch or saccharides. The beneficial microorganism comprises one or random combination of bacillus subtilis, bacillus licheniformis, bee bifidobacterium, bifidobacterium asteroids, minimum bifidobacterium, bifidobacterium coryneforme, lactobacillus jensenii, lactobacillus amylovorus, lactobacillus plantarum, tiny lactobacillus and lactobacillus bifermentans; and a gram of the beneficial microorganism comprises 10<9> to 5*10<9> viable bacteria. The preparation for preventing and controlling bee fungal diseases is applied to prevention and control of bee or silkworm fungal diseases.

The invention provides a synthesis method of stable isotope deuterium labeled 2-methyl-4-isothiazol-3-one, the synthesis method comprises the following steps: step 1, taking 3,3'-dimercaptodipropionicacid and thionyl chloride as raw materials, and obtaining 3,3'-dimercaptodipropionyl chloride through catalytic reaction by a catalyst; step 2, after an alkali and a carbonate are sequentially addedto deuterated methylamine hydrochloride, adding the 3,3'-dimercaptodipropionyl chloride obtained in the step 1 to react to obtain deuterated amide; step 3, adding a reaction solvent and sulfonyl chloride to the deuterated amide obtained in the step 2, continuously stirring the reaction system at 0 DEG C for reaction for 1 hour, and then continuously stirring and reacting at room temperature for 15hours to obtain the stable isotope deuterium labeled 2-methyl-4-isothiazol-3-one, wherein the molar ratio of deuterated amide to sulfonyl chloride is 1: 3. According to the invention, the reaction yield can reach 34%, the purity of the target product can reach 98%, and the deuterium generation rate can reach more than 99%.

The invention relates to the technical field of pesticide organic synthesis, and provides a saflufenacil intermediate preparation method, which comprises: a), carrying out reaction on 2-chloro-4-fluoro-5-aminobenzoate and ethyl 4,4,4-trifluoroacetoacetate to obtain an intermediate (1); b), reacting the intermediate (1) with methylamine hydrochloride to obtain an intermediate (2); and c), reactingthe intermediate (2) with an acylation reagent to obtain the 2-chlorine-4-fluorine-5-(3-methyl-2, 6-diketone-4-trifluoromethyl-2, 3-dihydropyrimidinyl-1(6H)- group) benzoate. The method solves the problems that toxic reagent raw materials with great harm are used in the existing saflufenacil intermediate reaction process, the operation is complicated, and the yield is not high.

The invention discloses a 2-[(2R, 6S)-6-[(2S)-2-hydroxy-2-phenethyl]-1-pipecoline]-1-hypnone synthesis method, and belongs to the field of organic synthesis. (1S, 2S)-1, 2-diphenyl diaminoethane serving as a raw material is subjected to acylation, substitution and the like to prepare chiral amine catalysts. A main route totally includes two steps: synthesizing glutaraldehyde, benzoyl acetic acid and methylamine hydrochloride to form cis-lobelanine; performing asymmetric selective reduction synthesis of 2-[(2R, 6S)-6-[(2S)-2-hydroxy-2-phenethyl]-1-pipecoline]-1-hypnone under mild reaction conditions and under the action of the catalysts. The raw material in the whole process route is cheap and easy to obtain, the catalysts can be recycled and can continue to be used, and the synthesis method is low in cost, simple in process, mild in reaction condition, convenient in operation and high in total yield.

Production of N-methyl-3,5-bistriflumethylaniline is carried out by oximation reacting 3,5-bistriflutoluyl aldehyde with methylamine hydrochloride, catalyzing and reducing the products. It yields more and is cheap.

The invention discloses a method for synthesizing [<2>H3]-1-methylamino-2-phenylpropane. The method is characterized by comprising the following steps: (1) subjecting phenylacetone, deuterated methylamine and tetraalkyl titanate or phenylacetone, deuterated methylamine, tetraalkyl titanate and an acid binding agent or phenylacetone, deuterated methylamine hydrochloride and tetraalkyl titanate to areaction, so as to obtain a first intermediate; (2) subjecting the first intermediate obtained in the step (1) and a reduction reagent to a reaction; (3) adding ammonia water into the step (2) for aquenching reaction, carrying out suction filtration to remove precipitates, carrying out precipitation with an organic solvent, merging liquid, and carrying out extraction and knockout to collect an organic phase, thereby obtaining the [<2>H3]-1-methylamino-2-phenylpropane. The method has the advantages that the synthesis route is short, the operation is simple and safe, the reaction time is short, and the yield exceeds 50%. Through further purification, both the purity and deuterated rate of the [<2>H3]-1-methylamino-2-phenylpropane can reach 99.5% or more, and thus, the [<2>H3]-1-methylamino-2-phenylpropane completely can serve as a deuterated internal reference substance for a mass-spectrum internal reference quantitative analysis method.

The invention discloses a synthetic method of a piperazidines drug intermediate. The synthetic method comprises the following steps: step one, reacting diethanol amine with thionyl chloride to prepare di(2-chloroethyl) methylamine hydrochloride; step two, reacting 3-chloroaniline with di(2-chloroethyl) methylamine hydrochloride to prepare 1-(3-chlorphenyl) piperazine hydrochlorid; step three, reacting 1-(3-chlorphenyl) piperazine hydrochloride with 1-bromine-3-chloropropane to prepare 1-(3-chlorphenyl)-4-(3-chloropropyl) piperazine hydrochloride. The line is simple, convenient and easy to perform, the aftertreatment operation is also greatly simplified, the reaction conditions are mild, and the product purity is high.

The invention provides a 1-(5-(2-fluorophenyl)-1-3-(3-methoxypropoxy)benzenesulfonyl chloride)-1H-pyrrol-3-yl)-N-methylamine salt type. The salt type contains organic acid salt and inorganic acid salt. By mainly screening various organic acids and inorganic acids, 1-(5-(2-fluorophenyl)-1-3-(3-methoxypropoxy)benzenesulfonyl chloride)-1H-pyrrol-3-yl)-N-methylamine hydrochloride and 1-(5-(2-fluorophenyl)-1-3-(3-methoxypropoxy)benzenesulfonyl chloride)-1H-pyrrol-3-yl)-N-methylamine fumarate which have relatively high purities and relatively good stabilities can be obtained and can be used for treating erosive esophagitis, gastric ulcer, duodenal ulcer and helicobacter pylori, eradicating adaptation diseases and treating relevant diseases caused by hyperacidity.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a temozolomide intermediate compound. According to the preparation method, 5-amino-1H-imidazole-4-nitrile is taken as an initial raw material and reacts with N, N '-carbonyldiimidazole, and the new temozolomide intermediate 5-amino-1-(1H-imidazole-1-carbonyl)-1H-imidazole-4-nitrile is obtained. Meanwhile, the invention provides a method for preparing temozolomide by using the novel intermediate compound. The method comprises the following steps: reacting 5-amino-1-(1H-imidazole-1-carbonyl)-1H-imidazole-4-nitrile with methylamine hydrochloride, diazotizing the obtained product, cyclizing, and hydrolyzing cyano to obtain temozolomide. The synthesis method of the novel intermediate provided by the invention is simple, the reaction of the novel intermediate and methylamine hydrochloride can effectively avoid the use of a highly toxic reagent methyl isocyanate and methylamino formyl chloride with higher toxicity and irritation, diazotization and ring-closure reaction are realized in one step, and the separation of unstable diazonium salt is avoided. The synthetic route is short, the yield is high, the reaction condition is mild, the process is stable, and the method is suitable for large-scale industrial production.

The invention discloses a laminine ester bromo oxamide derivative with anticancer activity and a composition thereof. The preparation method includes the steps of conducting backflow on laminine hydrochloride in thionyl chloride, adding methyl alcohol to conduct backflow again, steaming excess solvent, and regulating to neutral until white precipitate is dissolved out; filtering, using glacial alcohol and diethyl ether to wash, and conducting vacuum drying to obtain a white solid product; dissolving N-(5-bromine-2-hydroxyl aniline) ethyl oxalyl in an absolute ethyl alcohol solution, slowly adding drop by drop into anhydrous THF which dissolves prepared 6-N,N,N-trimethyl-2-carbamyl methylamine hydrochloride, conducting temperature reaction, and regulating the solution to neutral with dilutehydrochloric acid or a dilute hydrobromic acid solution until white precipitate is dissolved out; filtering, taking the precipitate to conduct recrystallization with ethyl alcohol, and conducting vacuum drying to obtain a target product. According to the laminine ester bromo oxamide derivative with anticancer activity and the composition thereof, through the introduction of a brominated ring structure, the cytotoxic activity of laminine to tumor cell strains in vitro can be enhanced.

The invention discloses a preparation method of an isavuconazonium sulfate intermediate. The preparation method comprises the following steps: firstly, reacting absolute ethyl alcohol, sodium ethoxide and methylamine hydrochloride, cooling an obtained reaction solution, adding an ethanol solution of 1-chloroethyl methylcarbamate for continuous reaction, and conducting filtering to obtain an ethanol solution of methyl carbamic acid-1-chloroethyl ester; cooling the obtained solution, adding an ethanol solution of 2-chloro-3-pyridinemethanol for stirring reaction, filtering a reactant, removing ethanol, adding dichloromethane for dissolving, conducting washing after dissolving, and taking an organic phase, namely a dichloromethane solution of 1-chloro-ethyl (3-hydroxymethyl-pyridin-2-yl)-methylcarbamate; and firstly adding BOC-sarcosine into the obtained solution, then adding carbodiimide and 4-dimethylaminopyridine in batches for a reaction, and performing treatment after the reaction, so as to obtain the isavuconazole onium sulfate intermediate. The isavuconazonium sulfate is prepared by using the technical scheme of the invention, the side reaction of the process is less, and the purity of the obtained product is high.

The invention belongs to the technical field of chemical synthesis, and particularly relates to a preparation method of optically pure lobeline hydrochloride and an enantiomer of the optically pure lobeline hydrochloride. According to the method, benzoylacetic acid, methylamine hydrochloride and glutaraldehyde are used as raw materials, and a target product can be prepared through condensation, reduction, acylation, resolution, oxidation and hydrolysis reactions in sequence. According to the method, meso-racemic lobeline is derived into raceme through acylation by adopting a desymmetry strategy, so that conditions are created for further resolution, and the use of a chiral catalyst which is high in price and tedious in preparation is avoided. In the splitting step, the product is filtered, the obtained filtrate is subjected to hydrolysis and other treatments to obtain an intermediate compound II, and the intermediate compound II can be recycled, so that the process cost is greatly saved; and moreover, the whole preparation process flow is simple to operate, mild in condition, high in optical purity of the product and very suitable for large-scale industrial production.

The invention discloses a preparation method of Dapagliflozin isomer impurities I. The preparation method comprises the following steps that a, 2-chlorine-5-bromobenzoic acid is dissolved in a first solvent; an acylation reagent is added; reaction is performed for 1 to 8h at 20 to 60 DEG C to generate a compound A; b, methoxyl methylamine hydrochloride is dissolved in a second solvent; alkali is added at -10 to 10 DEG C; then, the compound A capable of being dissolved in the second solvent is dropwise added; the temperature is maintained; stirring reaction is performed for 1 to 4h to obtain acompound B; c, a compound C is dissolved in a third solvent; a hexane solution of n-butyllithium is added at -78 DEG C; then, the compound B capable of being dissolved in the third solvent is dropwiseadded; after reaction, treatment is performed to obtain the Dapagliflozin isomer impurities I. The carbonyl substitution reaction is used, so that the reaction is exclusive; by-products are few; theoperation is simple; the process is stable; the repeatability is high; the total yield of the product is improved by 90 percent or higher; the cost is reduced; the commercialized production and the batch supply are facilitated.