58 results about "Hexahydropyridine" patented technology

The invention discloses a synthesis process of vecuronium bromide. The synthesis process comprises the following steps: generating epiandrosterone sulfonyl ester (III) by carrying out esterification reaction between epiandrosterone (II) and paratoluensulfonylchloride; generating 5Alpha-androst-2-alkene-17-ketone (IV) by carrying out elimination and dehydration reaction between the (III) and 2,6-lutidines; generating 17-acetoxyl-5Alpha-androstane-2,16-diene (V) by carrying out enolization and esterification reaction between the (IV) and isopropenyl acetate; generating (2Alpha, 3Alpha, 16Alpha,17Alpha)-diepoxy-17Beta-acetyl-5Alpha-androstane (VI) by epoxy reaction of the (V) under the effect of hydrogen peroxide; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha-hydroxyl-17-ketone (VII) by ring-opening and addition reaction of the (VI) under the effect of hexahydropyridine; generating 2Beta, 16Beta-di(1-piperidyl)-5Alpha-androstane-3Alpha,17Beta-diol (VIII) by the (VII)under the reduction of potassium borohydride; generating 2Beta, 16Beta-di(1-piperidyl)-3Alpha, 17Beta- acetoxyl-5Alpha-androstane (IX) by carrying out esterification reaction of the (VIII) under the acetylation of acetic anhydride; and generating vecuronium bromide (I) by carrying out quaternary ammonium salt reaction between the (IX) and bromomethane. The invention has the advantages of low cost,less pollution and high yield.

Provided herein are methods for treating levodopa-induced dyskinesia by administering to a subject (S)-2-amino-3-methyl-butyric acid (2R,3R,11bR)-3-isobutyl-9, 10-dimethoxy-1,3,4,6,7,11b-hexahydro-2H-pyrido[2,1-a]isoquinolin-2-yl ester, or an isotopic variant thereof, or a pharmaceutically acceptable salt or polymorph thereof.

The present invention provides a medical adhesive which has the advantages of short adhesion time, good flexibility of adhesive layer, sufficient hemostasis, high adhesion strength and short break-off time. The invention is characterized in that the medical adhesive is manufactured by the following inventive formula and technique, wherein the inventive formula is as follows: 30-75 parts of alpha-isobutyl cyanoacetate by weight, 3.5-23.5 parts of formaldehyde by weight, 0.15-1.55 parts of polymerization inhibitor by weight, 0.1-15.5 parts of pH adjusting agent by weight, and 0.5-19.3 parts of stabilizing agent. The inventive technique comprises the following steps: executing polycondensation reaction with alpha-isobutyl cyanoacetate, formaldehyde and hexa-hydrogen pyridine as pH adjusting agent, executing suction-filtering to the product after water cleaning, and vacuum drying; adding the material which is executed with vacuum drying in a fractionating flask, then adding phosphoric acid as pH adjusting agent, tricresyl phosphate as stabilizing agent and hydrochinone as polymerization inhibitor, mixing to uniform, installing a capillary tube of SO2 protective gas, starting depolymerization, distilling, collecting the component with constant boiling point, and packaging or pouring-in. The medical adhesive can be applied to the aspects of medicine, health-care, beauty treatment, daily life, etc.

The invention relates to a cefodizime sodium compound and a synthetic method thereof; the synthetic method comprises the step that cefodizime acid reacts with sodium acetate to obtain the cefodizime sodium; the synthetic method also comprises the step that cefotaxime acid reacts with 2-sulfydryl-4-methyl-5-thiazole acetic acid in a hexahydropyridine aqueous solution to produce the cefodizime acid; and the synthetic method of the cefodizime sodium compound has the advantages of simple operation, high yield up to 80 percent and high product purity more than 99.6 percent, thus obtaining surprising technical effects.

The invention belongs to the field of adhesives, and particularly relates to a synthesis technique of an alpha-cyanoacrylate monomer, which comprises the following steps: (1) directly reacting cyanoacetate and polyformaldehyde, which are used as raw materials, under solventless conditions by using a basic catalyst; (2) naturally cooling, keeping the temperature, and dehydrating to obtain the crude product; and (3) in the presence of a polymerization inhibitor, preparing the alpha-cyanoacrylate monomer, wherein the basic catalyst in the step (1) is one or mixture of hexahydropyridine, pyridine and KOH, the cyanoacetate is one or mixture of methyl cyanoacetate, ethyl cyanoacetate and n-butyl cyanoacetate, the polymerization inhibitor in the step (3) is hydroquinone and sulfur dioxide, a dehydrating agent is used for dehydration in the step (2); and the dehydrating agent is one or mixture of benzene, methylbenzene and methanol. The reaction process has the advantages of no need of organic solvent, low energy consumption, obvious environmental protection effect and high target product yield.

The present invention relates to an indolinospirobenzoxazine compound, its synthesis method and application. Said synthesis method includes the following steps: under the protection of nitrogen gas dissolving I-(R1)-2,3,3-trimethyl-pseudoindole iodine salt in anhydrous ethyl alcohol adding hexahydropyridine whose concentration is 0.5 wt%-10 wt% catalyst quantity, under the condition of refluxing drop-adding anhydrous ethyl alcohol solution of 2-nitroso-phenol derivative or 2-nitroso-3-R3-5-R2-phenol which is identical to 1-(R1)-2,3,3-trimethyl-pseudoindole iodine salt in gram molecular weight, drop-adding while distilling, after drop-addition continuously refluxing, concentrating, making the above-mentioned silicon gel column so as to obtain the invented product which can be used for making photochromic materials.

The invention provides a preparation method of thiofide DPTT-6, and relates to the technical field of thiofide. The preparation method comprises the steps of adding sulphur, hexahydropyridine and a surface active agent into a low-carbon alcohol solvent, mixing uniformly, then sequentially dropwise adding carbon disulfide and hydrogen peroxide, rising temperature for reaction, and preparing to obtain the thiofide DPTT-6. According to the preparation method, low-carbon alcohol low in toxicity, cheap in price and easy to recover and use indiscriminately is adopted as the solvent, and through theoxidation of the oxidizing agent hydrogen peroxide at lower temperature, dipentamethylenethiuram hexasulfide is synthesized. The preparation method has the advantages of simple process, high product yield and high purity; the prepared product has the product yield being larger than or equal to 97.0 percent, the initial melting point being larger than or equal to 115.0 DEG C, and the purity being larger than or equal to 98.0 percent; meanwhile, during the preparation process, no 'three wastes' (waste water, waste gas and waste solid) is discharged, all solvents are recovered and used indiscriminately, no environment pollution is caused, and zero emission of pollution is realized.

The present invention discloses a kind of L-menthyl chloroformate synthesizing process. Under room temperature and in the presence of catalyst, L-menthol and triphosgene are chloroacylated to obtain L-menthyl chloroformate. The process has reaction temperature of 25 deg.c, reaction time of 10-12 hr and catalyst pyridine, triethylamine or hexahydropyridine. The present invention has the advantages of substituting phosgene with less toxic solid triphosgene, easy control of the reaction, and relatively high safety and environment friendship.

The invention relates to a synthesis method of mepiquat chloride serving as a plant growth regulator, in particular to a method for synthesizing high-purity mepiquat chloride serving as a plant growth regulator with a one-step method. A process of the method comprises the following steps of: (1) dissolving a certain amount of hexahydropyridine into ethanol, and adding a certain amount of K2CO3; (2) adding methyl chloride into a system, wherein the weight ratio of the methyl chloride to the hexahydropyridine is 2:1-2.2:1; (3) filtering the system reacted in the step (2) to obtain KHCO3 and a mepiquat chloride system respectively, calcining the KHCO3 to obtain K2HCO3, and recycling the K2HCO3; and (4) removing ethanol from the mepiquat chloride system by evaporating to obtain high-purity mepiquat chloride, wherein the ethanol can be recycled. According to the method, high-purity mepiquat chloride can be synthesized with the one-step method, and the used K2CO3 and ethanol can be recycled. The process is easy to operate, is economical, has low cost and high mepiquat chloride purity, and can hopefully become a novel process for synthesizing high-purity mepiquat chloride serving as the plant growth regulator with the one-step method.

The invention discloses a preparation method of a silver-modified phosphorus-tungsten oxygen cluster catalyst. According to the method, silver nitrate, an organic ligand 4,6-di(pyridine-2-yl)pyrimidine-2-amine, phosphotungstic acid and dimethyl sulfoxide are put into a beaker to react, and after the reaction is finished, filtration is carried out, and the filtrate is slowly volatilized to obtain crystals of the silver-modified phosphorus-tungsten oxygen cluster catalyst. The method provided by the invention has the characteristics of high reaction speed, simple reaction process, high purity ofan obtained product, simple post treatment and the like. Moreover, in catalysis of a one-pot reaction of phenylacetylene, formaldehyde and hexahydropyridine, the conversion rate is as high as 99%, and the selectivity is as high as 100%.

The present invention relates to a kind of preparation method of rubber vulcanization accelerator bispentamethylene thiuram tetrasulfide, wherein said method uses water as solvent, and the raw materials used and their molar ratio are: hexahydropyridine: carbon disulfide: sulfur: hydrogen peroxide =1: 1~1.3: 1.8~2.5: 0.4~0.7, the specific process of the method is: under normal pressure, add hexahydropyridine and sulfur successively in the reaction kettle filled with water under stirring state, after adding Finally, control the temperature within the range of 20°C to 30°C, then add carbon disulfide liquid dropwise, and control the dropwise addition time for 2 to 3 hours. After the dropwise addition, measure the pH value of the reaction solution. After the temperature is stable within the range, control the temperature of the reaction solution at 30°C to 40°C, and start to add hydrogen peroxide dropwise to carry out the oxidation reaction. The oxidation reaction time is 3 to 4 hours; The liquid is separated, and the obtained solid is dried, crushed, sieved, and packaged to obtain the product. The method of the present invention has short production cycle, high safety factor, almost no waste gas emission, high melting point, good appearance and high yield of the obtained product, which is obviously superior to other preparation methods, and the comprehensive cost is low. Adopting the method of the present invention can improve the product Quality, energy saving and consumption reduction, reducing "three wastes" pollution.

The invention relates to a preparation method of a compound clopidogrel represented in the formula I and salts thereof, which comprises the following steps of: firstly, reacting methyl (R)-o-chloromandelate with thionyl chloride to obtain alpha-chloro-(2-chlorphenyl) methyl acetate, and condensing with 4,5,6,7-thiophane and [3,2c] hexahydropyridine hydrochloride in a solvent under alkaline catalytic action to produce the clopidogrel. The clopidogrel and salts thereof can be applied to medicines for inhibiting platelet aggregation.

The invention discloses an essence for trapping mosquitoes and flies. The essence for trapping mosquitoes and flies is prepared from, by mass permillage, 15 parts of 9,12,15-ctadecatrienal, 18 parts of methyl 2-fluorobenzoate, 18 parts of D-sorbitol, 10 parts of p-hydroxyphenethyl alcohol, 20 parts of pinane, 30 parts of isoeugenol and the like. P-methylphenol, benzpyrole, androsterone, hexahydropyridine (piperidine), molecular carboxylic acid and the like are added to the essence. The essence can effectively trap injurious insects and also has the important technical advantage that no chemical pollution is produced.

This invention relates to the preparation method of 3 -methylamino- piperidine which is key intermediate of broad spectrum antibiosis type balofloxacin. The invention takes 3 - halogenated pyridine as raw material, takes catalytic ammoniation and catalytic reduction to gain product.

A process for preparing 6-nitroindoline benzospiropyranium includes such steps as dissolving 5-nitrothio salicyladehyde and 1,2,3,3-tetramethyl indoline iodide in absolute alcohol, adding hexahydropyridine as catalyst, reflux reaction, concentrating, filtering and drying.

The invention discloses attractant with animal intestine odor and a preparation method thereof. The attractant with the animal intestine odor comprises the following raw materials in parts by weight: 30-50 parts of animal intestine hydrolysates, 0.5-3 parts of hexahydropyridine, 0.5-3.5 parts of trimethylamine, 5-10 parts of urea, 0.01-0.1 part of santal aldehyde, 0.1-1 part of limonitum; 0-4 parts of indole; 0.5-1.5 parts of liquid ammonia, 0-3 parts of cysteine hydrochloride; 0-30 parts of dextrine, and 15-50 parts of water. The attractant with the animal intestine odor has extremely strong stimulation effects on the smell sense and the taste sense of the livestock and the poultry, so that the attractant is capable of promoting food intake, improving food intake rate, as well as solving the problem of waste of the animal intestines as a resource; moreover, the attractant is mellow, stable and free of irritation in flavor, as well as good in attracting effect.

The invention relates to a method for synthesizing a fluoro nitrogen heterocyclic compound. In the method, a fluorine-containing hexahydropyridine compound is obtained with high selectivity through olefin fluoronation and amination which are performed in the presence of a metal catalyst by starting from simple nitrogen-containing olefins and using a hypervalent iodine compound as an oxidant and an inorganic fluoride as a fluorine source.

The invention discloses an epoxy coating with good heat stability and high adhesive force. The epoxy coating comprises a main material and an auxiliary material, wherein the weight ratio of the main material to the auxiliary material is 10:(3-5). The main material is prepared from, by weight, 10-20 parts of epoxy acrylate resin, 25-40 parts of bisphenol A epoxy resin, 5-8 parts of silicon carbide micropowder, 1-3 parts of mica iron oxide, 3-7 parts of graphene nano-sheets, 5-12 parts of lignin, 4-8 parts of blanc fixe, 5-15 parts of modified hyaluronic acid, 1-2 parts of 3-amino propyl triethoxy silane, 1-3 parts of dispersant and 20-60 parts of water. The auxiliary material is prepared from, by weight, 1.8-2.2 parts of acetic ether, 5-8 parts of diamine methyl cyclohexane, 10-20 parts of cyclohexane and 20-30 parts of water. The epoxy coating has excellent mechanical performance, good corrosion resistance and heat stability and high adhesive force.

The present invention relates to relates to 9, 10-dihydro anthracene chromophore compound and its preparation. The preparation process includes the following steps: introducing two formyls with 1, 1-dichloromethyl ether as formylation reagent to the methoxyl para position of the material 1, 8-dimethoxyl-9, 10-dihydro anthracene under the catalysis of Lewis acid and titanium tetrachloride to obtain 4, 5-dimethoxyl-1, 8-diformyl-9, 10-dihydro anthracene; and the reflux reaction between 4, 5-dimethoxyl-1, 8-diformyl-9, 10-dihydro anthracene and isophorone -malononitrile condensate or isophorone -barbituric acid condensate in absolute alcohol as solvent in the catalysis of hexahydropyridine and acetic acid to obtain the organic compound. The compound of the present invention has high second-order non-linear coefficient and excellent transmittancy and may be used as second-order non-linear optical material, especially laser frequency doubling material.

The invention belongs to the technology field of medical treatment, and relates to component of liquid 'band-aid'. The liquid band-aid contains 94% ethylene glycol monoethyl ether cyano-acetic acid, 36% formaldehyde aqueous solution, basic catalyst (2% hexahydropyridine aqueous solution), 85% phosphoric acid, phosphorus pentoxide, 99% hydroquinone, tricresyl phosphate, and dispersant (sodium dodecyl benzene sulfonate). The liquid band-aid is characterized in that the liquid band-aid has hemostatic, analgesic, wound surface protecting, wound infection preventing, and wound healing effects; when in use, the band-aid liquid instantly diffuses into affected part to form a protective film, instantly seals the wound surface to block invasion of bacteria or foreign matter, and is water-resistant. The liquid band-aid has rapid bonding effect (5s-13s) for small-area open surgery wound, which replaces cuticular suture; and has non-toxicity, no bacteria, and no irritation and allergy to skin.

The invention discloses a synthetic method of a benzamidine compound. The synthetic method comprises the following steps of: taking the formanilide as the raw material, adding phosphorus oxychloride and an acid-binding agent triethylamine or diisopropylamine, and reacting to obtain corresponding isonitrile, directly adding Cu2O and diethylamine, or Cu2O and piperidine to the reaction liquid directly without separation, continuing to react, standing the reaction liquid for layering, extracting the oil layer, extracting the obtained water layer by using ethyl acetate and then extracting the oil layer, blending the two oil layers obtained and removing the ethyl acetate through spiral flashing, carrying out column chromatography, removing a solvent through spiral flashing, thus obtaining an oily liquid at last, namely the benzamidine compound. The synthetic method is simple in reaction process and moderate in reaction conditions, and the yield of the synthetic method is above 70%.

The invention discloses a preparation method of curcumin derivatives, and an antitumor drug. The preparation method comprises the steps of: weighing curcumin to be dissolved into methanol-chloroform mixture solution, and dropwise adding hexahydropyridine as a catalyst; dropwise adding furan formaldehyde methanol solution under stirring, reacting at room temperature, and standing; filtering to retain precipitation product, washing with petroleum ether to remove unreacted active ingredients, and drying; concentrating the filtered mother liquor, washing the reaction liquid with water, separating out the product, filtering to obtain precipitation, washing with petroleum ether, filtering and drying; combining to obtain the product, placing the chloroform-methanol mixture solution for recrystalization, and drying the product to be constant-weight. The new curcumin derivatives synthesized by structure improvement of two curcumin derivatives: 4-(2-fural) curcumin and hydrazinobenzoic acid curcumin which are synthesized by adopting the preparation method of curcumin derivatives is good in water solubility, slow in in-vivo metabolism, high in bioavailability, and higher in activity, and has important application prospects.

The present invention relates to synthesis process of 4-(1, 5-dimethyl-1-vinyl-4-hexenyl) phenol, normally named as antifeedant, and the synthesis process is superior to available ones. The synthesis process has geraniol as main material and includes the reaction with vinyl ethyl ether, Claisen rearrangement reaction to obtain 3-vinyl-rhodinal, reaction with hexahydropyridine, enamiation, conjugate addition with methyl vinyl ketone and cyclization and condensation to 4-(1, 5-dimethyl-1-vinyl-4-hexenyl)-2-cyclohexene ketone, and dehydrogenation to obtain the product 4-(1, 5-dimethyl-1-vinyl-4-hexenyl) phenol. The present invention uses natural product as main material, and has simple reaction process, high selectivity and high yield.

The invention belongs to the field of medical technology, relating to a new diketone piperazidine-like derivative and application thereof, specifically relating to a new diketone piperazidine-like derivative capable of treating tumor diseases. The structural formula of the compound is shown in the figure I and the figure II; n can be 0, 1, 2; the base group R can be amino-group, ethylamino group, tri-amino, abnormal tri-amino, fourth amino, abnormal fourth amino, tertiary butyl amino, circular tri-amino, circular fifth-amino, hexamethylene amino, dimethyl amino, diethylin, tetralin pyrrolyl, hexahydropyridine group, 4-methyl hexahydropyridine group, morpholinyl, piperazine group, and nitrogen methyl piperazine group. The compound has stable and definite structure, and the anti-tumor activity experiments show that the compound has very strong antitumor activity and has the advantages of strong active activity, small dosage, and the like. The diketone piperazidine-like derivative can be made into preparation for treating tumor diseases.

The invention provides a dihydro-pyrazolo hexahydropyridine derivative and a preparation method thereof. The method comprises the following steps of: performing Michael addition reaction of substituted amine (a) and methyl acrylate to prepare N,N-bis(beta-methyl propionate) substituted amine (b); performing Dieckmann condensation of (b) under the action of sodium alcoholate and hydrolyzing and decarboxylating under the action of acid to obtain yellow oily matter N-substituted piperidine-4-ketone (d); reacting (d) and aromatic aldehyde to remove bimolecular water to obtain N-substitution-3,5-dibenzal piperidine-4-ketone (e); and performing reaction of (e) to form the dihydro-pyrazolo hexahydropyridine derivative. The preparation method is simple, and the dihydro-pyrazolo hexahydropyridine derivative is convenient to produce in large scale; and a lead compound of the prepared dihydro-pyrazolo hexahydropyridine new medicine has the obvious inhibitory activity on leukemia K562 cancer cellproliferation, and has the obvious practicality in the production of modern medicines.

The invention discloses a pipe processing cutting fluid, which is made by the following raw materials in parts by weight: 5-9 parts of titanium dioxide, 10-15 parts of whale oil sulfide, 3-8 parts of deionized water, 3-9 parts of sodium hypochlorite, 3-9 parts of barium carboxylate, and 3-8 parts of hexahydropyridine. Compared with the existing cutting fluid, the pipe processing cutting fluid has thixotropy, and can be transported to a work piece by a pneumatic pump or stirred into a liquid state from a paste state, so that the cutting fluid is easy to transport and use, and the consumption amount of the cutting fluid is reduced. The pipe processing cutting fluid has very high permeability, and is easy to clean.

The invention discloses a method for preparing 3-isobutylglutaric acid. The method includes the following steps: carrying out a Knoevenagel condensation reaction on isovaleraldehyde and diethyl malonate with hexahydropyridine acetate as a catalyst in a cyclohexane solvent; carrying out a heating decarboxylation reaction on a product obtained by the first step in a solution composed of sodium chloride, DMSO and water; carrying out a Michael addition and decarboxylation reaction on a product obtained by the second step and diethyl malonate in an alcohol solvent of an alkali; and carrying out a hydrolysis reaction on a product obtained by the third step under an acidic condition to obtain the 3-isobutylglutaric acid product. The method of the invention uses the cheap and easily available isovaleraldehyde and diethyl malonate as raw materials, overcomes the defect of large steric hindrance of carbon-carbon a double bond in 5-methyl-2-cyano-2-hexenoate in the prior art, shortens the reaction time, and increases the reaction conversion rate of the isovaleraldehyde, thereby ensuring the overall yield of the 3-isobutylglutaric acid product.

The invention creates and provides an environment-friendly automobile cleaning and glazing agent. The environment-friendly automobile cleaning and glazing agent comprises the following components in parts by weight: 10-30 parts of sodium silicate, 2-3 parts of hexahydropyridine, 4-6 parts of sodium valproate, 5-8 parts of potassium citrate, 1-5 parts of dimethylhydrazine, 10-20 parts of methyl bromoacetate, 3-4 parts of herba lycopi, 6-8 parts of clodronate disodium, 2-6 parts of tricarbon alcohol acid, 1-2 parts of tetrahydrofolate, 1-2 parts of tetrahydropyrane, 15-25 parts of sodium alginate, 1-2 parts of simvastatin, 4-8 parts of diethylenetriaminepentaacetic acid, 50-60 parts of ethanol, 1-3 parts of sodium oleate and 1-2 parts of clerodendrum inerme. The creation of the invention has the advantages and positive effects that the environment-friendly automobile cleaning and glazing agent has not only good cleaning and glazing effects, but also good environmentally friendly effect; components in the product have good degradation function and cannot cause harm to a human body and can simultaneously reduce environmental pollution.

The invention discloses a wood adhesive which consists of following components by weight portion: 1 portion of paraformaldehyde; 2 to 4.6 portions of ethylene dichloride; 3 to 4 portions of ethyl ester and / or 10 to 15 portions of hexahydropyridine; 0.03 to 0.54 portion of phosphoric anhydride and / or 0.022 to 0.514 portion of hydroquinone; 0.003 to 0.018 portion of paratoluenesulfonic acid; and less than 0.1 portion of additive; the preparation method includes the steps of preparing the finished product after a polymerization step, a pyrolysis step, a distillation step and a rectification step according to the components. The whole reaction system is always in back flow state during the preparation process, by methods of adding inhibitor and improving technical conditions etc. at the depolymerization stage of the reaction, the occurrence of side reaction is reduced, and properties such as purity etc. of the product is enhanced, thus allowing the invention to have the advantages of high adhesion speed, super penetrability, free from yellow discoloration and arching, as well as short curing time.