58 results about "Dimethylpiperidone" patented technology

The invention discloses a preparation method of tilmicosin. The method comprises the following steps of: reacting tylosin phosphate serving as a raw material with 3,5-lupetidine by taking alcohol as a solvent and taking anhydrous formic acid as a catalyst at 65-97 DEG C to obtain 20-dihydro-20-deoxy-(3,5-lupetidine-1-radical)tylosin serving as an intermediate; concentrating the solvent; and adding residues into 0.1N sulfuric acid solution for hydrolyzing to obtain tilmicosin, wherein the mass volume ratio of the tylosin phosphate to the alcohol is 1:(2-10), the mass ratio of the tylosin phosphate to the 3,5-lupetidine to the anhydrous formic acid is 1:(0.11-0.17):(5.6-8), and the mass volume ratio of the tylosin phosphate to the 0.1N sulfuric acid solution is 1:(2-6). The reaction formula is shown in the specifications. By adopting the method, the defects of the prior art can be overcome. The method is easy to control, and has high yield and low production cost.

Cosmetic or dermatological compositions which comprise at least one piperidinium salt, preferably a 4-[(2-cyclopentyl-2-hydroxyphenylacetyl)oxy]-1,1-dimethyl-piperidinium salt, and the use thereof, particularly as antiperspirants. This Abstract is neither intended to define the invention disclosed in this specification nor intended to limit the scope of the invention in any way.

The invention relates to a novel preparation method of a tofacitinib intermediate and in particular to a preparation method of the tofacitinib intermediate (3R,4R)-1-benzyl-N-4-dimethyl piperidine-3-amine dihydrochloride. The preparation method comprises the following steps of: by taking 1-benzyl-4-methyl-1,2,3,6-tetrahydropyridine as an initial raw material, oxidizing olefin to form a ketone II by means of a one-step process; forming imine III with amine; applying asymmetric reduction imine to form amine; removing a trans isomer by recrystallization to obtain a cis-form structure IV; and finally, applying chiral resolution to obtain a final product (3R,4R)-1-benzyl-N-4-dimethyl piperidine-3-amine dihydrochloride I. The preparation method is creative in process, the process steps are shortened, and the synthetic yield of an asymmetric compound is greatly increased, thereby laying a solid foundation for industrial production.

The present invention relates to a novel preparation method of a tofacitinib intermediate bis-(3R,4R)-1-benzyl-N,4-dimethyl piperidin-3-amine L-di-p-toluyl tartrate. According to the preparation method, 3-amino-4-methyl piperidine is adopted as a starting raw material, is subjected to a N-methoxycarbonylation reaction under the sodium hydride effect, and is subjected to a catalytic hydrogenation reaction, a nucleophilic substitution reaction, an amide reduction reaction under the red aluminum effect, and L-di-p-toluyl tartaric acid (L-DTTA) chiral splitting so as to finally prepare the target compound bis-(3R,4R)-1-benzyl-N,4-dimethyl piperidin-3-amine L-di-p-toluyl tartrate. The process of the present invention has characteristics of further existing process improving, simple operation, easy post-treatment, high yield, and low cost.

This invention provides a harmful organism control composition having an excellent harmful organism control effect and comprising as an effective ingredient the following 4-(2-butynyloxy)-5-fluoro-6-(3,5-dimethylpiperidino)-pyrimidine (X):and a hydrazide compound represented by formula (I):wherein A1 and A2 represent, for example, an oxygen atom; R1, R2, and R3 represent, for example, a hydrogen atom, a C1-6 alkyl group optionally substituted by a halogen atom; and Q represents, for example, a methoxycarbonyl group.

A method for making zeolite SSZ-35 is disclosed using a N,N-diethyl-2,3-dimethylpiperidinium cation or a N,N-dimethyl-2-isopropylpiperidinium cation as a structure directing agent.

The invention belongs to the technical field of pharmaceuticals, and discloses a method for synthesizing tilmicosin through low-quality tylosin. The method comprises the steps that tylosin tartrate and 3,5-dimethylpiperidine are subjected to an amination reaction by taking isoamyl acetate as solvent under the certain acidity and temperature conditions, acidic hydrolysis is conducted, hydrolysate passes through a Beta molecular sieve, impurities produced by a D component in tylosin are adsorbed, alkali adjustment and crystallization are conducted, and high-quality tilmicosin is obtained. According to the method for synthesizing tilmicosin through low-quality tylosin, low-quality tylosin tartrate can be adopted, the quality requirement of the raw material is lowered, the raw material cost is reduced, the applied Beta molecular sieve is easy to separate and capable of being recycled, economical efficiency and environmental protection are achieved, operation is easy, the method is suitable for industrial production, and the quality of the obtained product is superior to that of the product based on Pharmacopeia 2010.

The invention belongs to the field of medicinal chemistry, and discloses a 3, 6 modified-[1, 2, 4] triazole [3, 4-alpha] phthalazine compound having antitumor activity as well as a synthesizing method and application of the 3, 6 modified-[1, 2, 4] triazole [3, 4-alpha] phthalazine compound. The 3, 6 modified-[1, 2, 4] triazole [3, 4-alpha] phthalazine compound has a structure as shown in a general formula I, wherein R1 refers to H, methyl or phenyl; R2 refers to 4-fluorophenyl, 4-chloroanilino, 4-bromophenyl, 4-methoxyphenyl, 4-hydroxydiphenyl, 2-fluorophenyl, 3-trifluoromethyl)phenyl]amino, naphthylamine-1-yl, pyrrolidone-1-yl, piperidine-1-yl, 3,5-dimethyl piperidine-1-yl, morpholine-4-yl, or piperazidine-1-yl. The preliminary in-vitro antitumor activity finds that the serial compounds have obvious inhibit and killing effects on multiple tumor cells, and the 3, 6 modified-[1, 2, 4] triazole [3, 4-alpha] phthalazine compound can act as an active ingredient to be applied to clinical prevention and cancer treatment after being developed into a novel medicament.

The invention discloses a catalyst for continuously preparing 3,5-dimethyl piperidine. The catalyst is prepared from an activated carbon carrier, Ru, Rh and M, wherein the Ru, the Rh and the M are loaded on the activated carbon carrier, the mass percent content of the Ru in the catalyst is 1% to 5%, the mass percent content of the Rh is 0.05% to 1%, the mass percent content of the M is 0.05% to 1.5%, and the M is Pt, K, Ce or Sn. In addition, the invention further discloses a preparation method of the catalyst and a method for continuously preparing the 3,5-dimethyl piperidine. The catalyst disclosed by the invention has the characteristics of high activity, high selectivity and high stability and can can realize high-efficient catalysis to prepare the 3,5-dimethyl piperidine in high efficiency; the converting rate of a raw material of 3,5-dimethyl pyridine is 100%, the yield of a product of the 3,5-dimethyl piperidine is larger than 99%, and cis-trans isomerism ratio is (87 : 13) to ( 83 : 17).

The invention relates to the field of synthesis of catalytic materials and discloses a synthesis method and an application of an AEN-structured Si-P-Al molecular sieve. The synthesis method comprisesa mode one: a mixed solution containing a P source, an Al source, a Si source, a structure-directing agent and water is subjected to hydrothermal crystallization with a hydrothermal method and then issubjected to solid-liquid separation and dried; a mode two: a mixed solution A containing the P source, the Al source and water is aged and dried with a P-Al dry glue liquid phase conversion method,and dry P-Al glue is prepared; a raw material mixture B containing the dry P-Al glue, the Si source, the structure-directing agent and water is subjected to hydrothermal crystallization, solid-liquidseparation and drying, wherein the structure-directing agent is 1-methyl-4-piperidinone and / or 1,3-dimethyl-4-piperidone. According to the synthesis system, the AEN-structured Si-P-Al molecular sieveis easy to synthesize. The AEN-structured Si-P-Al molecular sieve synthesized with the method can be applied to storage of small molecule gases such as hydrogen, methane and the like, can also be usedfor gas absorption separation and has good application prospect.

The modified polycarbodiimide compound of the present invention is obtained by modifying a polycarbodiimide compound derived from a diisocyanate compound with at least one aliphatic amine selected from the group consisting of diethylamine, methylisopropylamine, tert-butylethylamine, di-sec-butylamine, dicyclohexylamine, 2-methylpiperidine and 2,6-dimethylpiperidine. The curing agent of the present invention comprises the modified polycarbodiimide compound of the present invention. The thermosetting resin composition of the present invention comprises a carboxyl group-containing resin having a carboxyl group in a molecule or an epoxy resin having two or more epoxy groups in one molecule, and the curing agent of the present invention. Thus, a modified polycarbodiimide compound that can allow a resin composition to be cured at a relatively low temperature and that can suppress curing of a resin composition in a drying step before a thermal curing step of a resin composition, a curing agent comprising the modified polycarbodiimide compound, and a thermosetting resin composition comprising the curing agent can be provided.

The invention discloses a polymerization inhibitor for a preparation apparatus of acrylic acid. The polymerization inhibitor contains 2,6-dimethylpiperidin-1-oxyl free radical and N,N'-dimethylthiourea, the mass ratio is 1:1-1.5, and the polymerization inhibitor is applied to a C2 acetic acid removing tower and / or a C2 return tank of the preparation apparatus of acrylic acid. The polymerization inhibitor is an environmental protection high-efficient polymerization inhibitor, and the polymerization inhibitor has the advantages of few usage amounts without toxicity and generation of corrosion; good polymerization inhibiting effects are provided, environment and occupational health of employees are protected, and the polymerization inhibitor accords with high efficient and environmentally friendly production and operation ideas.

The invention relates to a preparation method of high-purity cis-3,5-dimethylpiperidine, and belongs to the field of organic synthesis. According to the preparation method, 3,5-dimethyl pyridine is taken as a raw material, a 3,5-dimethylpiperidine crude product is obtained via catalytic hydrogenation, and high-purity cis-3,5-dimethylpiperidine is obtained via precipitation purifying, wherein the cis gas chromatographic purity is larger than 99.5%. in the preparation method, neutral aluminium oxide and an alkali are introduced, and the combination mode of pyridine molecules with catalyst molecules in hydrogenation process is changed, so that it is beneficial for formation of cis-form products, and the crude product which can be applied in drug production directly is obtained; the cis-isomeride with a purity higher than 99.5% after treatment is obtained for the first time in the field of cis synthesis and separation of 3,5-dimethylpiperidine, and great referential significance and relatively high commerical value in the fields of synthesis purification and industrialized production of piperidine derivatives are achieved.

A sustained release anti-cancer injection with edelfosine consists of the edelfosine with effective anti-cancer amount and an amphiphilic block copolymer hydrogel, wherein, part or the whole of the edelfosine is encapsulated in sustained release microsphere and exists singly in the form of the sustained release microsphere or microsphere and micro-powder in the sustained release injection. The amphiphilic block copolymer hydrogel is selected from PLGA-polyethylene glycol-PLGA, sustained release gel has temperature-sensitive gelation property; and the sustained release gel is flowable fluid in an environment below body temperature, and can automatically change into biodegradable and absorbable non-flowable water-insoluble gel in bodies of warm blooded animals, thus causing the drug to be slowly released in the local part of tumor; the sustained release microsphere is favorable to the stable and sustained release of the drug, the dual sustained release is beneficial to controlling tumor cells in dormancy stage, the drug in the form of the micro-powder in the sustained release gel is favorable to the relatively quick release, thus being beneficial to controlling cells with quicker proliferation. The sustained release anti-cancer injection with edelfosine can be used together with radiotherapeutic particles, chemotherapeutic drugs, etc.

Disclosed is a single step process for separating Cis-3,5-dimethylpiperidine from a mixture of its geometrical isomers. The method comprises hydrogenation of 3,5-lutidine in the presence of water and 5% ruthenium on alumina as the catalyst at a predetermined range of temperature and pressure and does not involve the use of any organic solvent.

The invention discloses a detection method of (3R, 4R)-1-benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride and an enantiomer thereof, which comprises the following steps: carrying out pre-columnderivatization on 1-benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride by using a chiral derivatization reagent isothiocyanate or isocyanate, and detecting by using high performance liquid chromatography. According to the method, (3R, 4R)-1-benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride and (3S, 4S)-1-benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride are separated, the detection cost is low, and the sensitivity, specificity and accuracy are good, so that the method is an effective detection method for controlling the quality of the tofacitinib citrate starting raw material, therefore, the tofacitinib citrate product quality and the medication safety of patients are further ensured.

The invention relates to a method for using tylosin D as a raw material to prepare tilmicosin. The method comprises the steps of using tylosin D as the raw material, oxidizing a C[20]position primary dydroxide radical into a formyl group through a selective oxidant to obtain a first midbody, then conducting hydrolysis and decarbonization on mycarose to obtain a second midbody, and making formic acid and 3,5 dimethyl piperidine subjected to a reductive ammonolysis reaction to obtain the product tilmcosin. According to the method for using tylosin D as the raw material to prepare tilmicosin, tylosin D is adopted as the raw material, through the specific selective oxidant, tylosin D is converted into an effective component in compound tilmicosin and is prevented from being converted into impurities, thus a new path is opened up for the preparation of tilmicosin, and the problems that the impurities are high in residual rate and the yield rate is low when tylosin is adopted as an original raw material to prepare tilmicosin are solved.

The present invention relates to crystalline forms of (9E,10E)-2,7-bis((3,5-dimethylpiperidin-1-yl)sulfonyl)anthracene-9,10-dione dioxime, pharmaceutical compositions comprising the crystalline form, processes for preparing the crystalline form and methods of use therefore.

The invention discloses a preparation method of a tofacitinib intermediate cis-1benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride. The synthetic method comprises the following steps: taking 3-bromo-4-methylpyridine as an initial raw material, performing substitution reaction with amine to obtain a compound III, and performing acetyl or tert-butyloxycarbonyl protection and catalytic hydrogenation on the compound III to obtain a piperidine compound V. The compound V and benzaldehyde are subjected to reductive amination or react with benzyl halide to obtain a compound VI. A protecting groupis removed from the compound VI, and a hydrochloride compound I. 2HCl is formed at the same time. The synthesis method is simple to operate, high in total yield, high in product purity, stable in quality and suitable for industrial production.

The invention discloses a synthesis method of a 3, 5-dimethyl piperidine onium salt template agent. The method comprises the following steps: synthesizing 1, 3, 5-trimethyl pyridine quaternary ammonium salt from chloromethane and 3, 5-dimethyl pyridine; under the action of a catalyst, carrying out hydrogenation reaction on the 1, 3, 5-trimethylpyridine quaternary ammonium salt to generate 1, 3, 5-trimethylpiperidine; reacting 1, 3, 5-trimethylpiperidine with dimethyl carbonate in a nitrogen atmosphere to generate a 3, 5-dimethyl piperidine onium salt with methyl carbonate radicals; and dissolving the 3, 5-dimethyl piperidine onium salt with methyl carbonate radicals in water, standing for layering, removing an organic phase in the raw material, taking a water phase, distilling, adding calcium hydroxide, reacting to obtain a 3, 5-dimethyl piperidine onium salt with hydroxide radicals asanions, and concentrating until the mass fraction of the 3, 5-dimethyl piperidine onium salt is 24-32% and the mass fraction of the hydroxide radicals is 3-4%. The invention also discloses a method for preparing a molecular sieve by adopting the 3, 5-dimethyl piperidine onium salt template agent.

The invention discloses a method for synthesizing a chiral tofacitinib citrate intermediate by an enzymic method. The method comprises the following steps: by taking 4-methyl-1-(phenyl methyl)-3-piperidone (TOF15) as a raw material, performing biological catalysis to obtain a chiral intermediate TOF 20-A, and then performing methylation reaction to obtain an intermediate TOF 25-A, namely free (3R, 4R)-1-benzyl-N, 4-dimethyl piperidine-3-amine, wherein the intermediate TOF 25-A can be further made into hydrochloride, so that (3R, 4R)-1-benzyl-N, 4-dimethyl piperidine-3-amine dihydrochloride (TOF30) can be obtained. The method is a synthesis technology which is low in cost, high in yield and environment-friendly, is suitable for large-scale industrial production, and has huge market application value.

The invention discloses a preparation method of N, N-dimethyl piperidine chloride salt. The method comprises the following steps: adding alkali liquor, a solvent and piperidine into a closed reactioncontainer, then introducing methyl chloride, and heating for reaction to obtain the N, N-dimethyl piperidine chloride salt. According to the method, the high-purity N, N-dimethyl piperidine chloride salt (with the content greater than 99%) can be synthesized; side reaction hardly occurs in the reaction process, SN2 main reaction is very thorough, and water can be separated from a reaction system;and the solubility of the N, N-dimethyl piperidinium chloride salt in the system is small at low temperature, and thus, the N, N-dimethyl piperidinium chloride salt is separated from the system favorably. The yield and content of the N, N-dimethyl piperidinium chloride salt are quite high; and the preparation method is safe to operate and low in cost.

The invention discloses a preparation method of trans-3,5-dimethylpiperidine, belonging to the technical field of chemical products. The method comprises the following steps: A, adding 3,5-dimethylpyridine, deionized water and a composite catalyst into a high-pressure reaction kettle for a reaction under the protection of hydrogen, and carrying out suction filtration after the reaction is finished to obtain a crude 3,5-dimethylpiperidine product; and B, cooling the crude 3,5-dimethylpiperidine product obtained in the step A to room temperature, taking out a reaction mixture, conducting standing, and taking supernatant liquid to obtain the trans-3,5-dimethylpiperidine. According to the invention, reaction conditions are mild and easy to control, reaction effect is good, and a trans content can reach 20-35%.

The invention relates to a making method and an application of a polythiophene derivative electrochemiluminescence sensor. In the invention, a polythiophene derivative poly(3-1,1'-dimethyl-4-piperidylmethylene)-2,5- chlorothiophene) is used as a luminescence material, has good water solubility and good optical performances, and is in favor of constructing sensitive and stable electrochemiluminescence sensors. Bromate ions are used as a coreactant of an electrochemiluminescence reaction of poly(3-1,1'-dimethyl-4-piperidylmethylene)-2,5- chlorothiophene) due to the oxidation of the bromate ions, and the electrochemiluminescence intensity varies with the concentration of the bromate ions in order to detect the bromate ions. The potassium bromate electrochemiluminescence sensor made in the invention has the characteristics of simplicity, rapidness and sensitiveness, and is suitable for the rapid detection of potassium bromate in drinking water and river water.

The invention relates to the field of pharmaceutical engineering, and particularly relates to a preparation method of tilmicosin. The preparation method comprises the following steps: taking tylosin tartrate and 3, 5-dimethylpiperidine as raw materials under a certain temperature condition, and enabling the tylosin tartrate and the 3, 5-dimethylpiperidine to generate a Mannich condensation reaction in a polar solvent medium to obtain an intermediate state substance; reducing the intermediate state substance to obtain an intermediate; and desugaring the intermediate to obtain tilmicosin. The preparation method overcomes defects that the tilmicosin preparation method in the prior art needs more catalysts, and the catalysts are easily doped into a product to cause lower purity. Therefore, compared with the prior art, in the invention, different synthesis routes are adopted, and the tilmicosin can be efficiently synthesized under a condition of omitting the catalysts; meanwhile, reaction time is effectively shortened so that production efficiency of tilmicosin is improved, and the purity of the synthesized tilmicosin is higher.

The invention belongs to the technical field of cotton production, and particularly relates to a cotton topping agent and preparation and application methods thereof. The cotton topping agent comprises the following components in percentage by mass: 35-45% of a first component and 55-65% of a second component, wherein the first component is 2-chloroethyl trimethyl ammonium chloride and / or N, N-dimethyl piperidine ammonium chloride; the second component is carbamoyl ethyl phosphate ammonium salt and / or N-(2-chloro-fluorobenzyl)-N-ethyl-alpha, alpha, alpha-trifluoro-2, 6-dinitro-p-toluidine, andthe result shows that the chemical topping agent is suitable for an environment with high temperature, much rainwater and high humidity, and can obviously reduce the plant height of newly born main stems and fruit branches of cotton and increase the boll number of a single plant; the chlorophyll content of leaves is increased, and the photosynthetic intensity is remarkably enhanced; the falling rate of cotton buds and bolls is reduced, and the seed cotton yield is increased; and labor investment can be saved by more than 0.5 per mu.

Provided are a novel process for preparing (3R,4R)-1-benzyl-N,4-dimethylpiperidin-3-amine or a salt thereof, which is an intermediate useful for the preparation of tofacitinib, an intermediate used in the process, i.e., isopropanol solvate of methyl ((3R,4R)-1-benzyl-4-methylpiperidin-3-yl)carbamate dibenzoyl-L-tartrate, an intermediate, having excellent stability, useful for the preparation of tofacitinib, i.e., (3R,4R)-1-benzyl-N,4-dimethylpiperidin-3-amine acetate, and a process for preparing tofacitinib or a pharmaceutically acceptable salt thereof.