129results about How to "Reasonable process conditions" patented technology

The invention discloses a method for preparing 2,5-dimethyl phenylacetic acid. The 2,5-dimethyl phenylacetic acid is a fine chemical engineering intermediate which is widely applied in fields of medicines and pesticides, and particularly is a key intermediate of spirotetramat serving as a novel insecticide. The method comprises the following steps of: mixing paraxylene serving as a raw material and ionic liquid serving as solvent with paraformaldehyde and concentrated hydrochloric acid, and performing a chloromethylation reaction to obtain 2, 5-dimethyl benzyl chloride; and performing a carbonylation reaction and a hydrolysis reaction of the 2, 5-dimethyl benzyl chloride and an acid-binding agent and the solvent in a reactor under the action of a catalyst to obtain the 2,5-dimethyl phenylacetic acid. The method has a novel process, short synthetic reaction steps, simplicity of operation, low production cost, high reaction yield, and environmental friendliness, and is suitable for industrial production.

The invention discloses a method for preparing lenalidomide. The method comprises the following steps: firstly, etherifying 2-methyl-3-nitrobenzoic acid to obtain 2-methyl-3-nitrobenzoic acid methyl ester, brominating to obtain 2-brooethyl-3-nitrobenzoic acid methyl ester, reacting L-glutamine and tert-butyl dicarbonate to obtain N-Boc glutamic acid, acquiring 3-amino-2,6-piperidine diketone protected by Boc from N-Boc-glutamic acid in the presence of a condensing agent and a catalyst, further reacting with acid to prepare 3-amino-2,6-piperidine diketone hydrochloride, reacting 3-amino-2,6-piperidine diketone with 2-brooethyl-3-nitrobenzoic acid methyl ester so as to obtain 3-(4-nitryl-1,3 dihydro-1-oxo-2 hydrogen-isobenzazole-2-yl) piperidine-2,6-diketone, and finally reducing, thereby obtaining lenalidomide. The method disclosed by the invention is high in product yield.

The invention discloses a novel preparation method of an asenapine intermediate, comprising the following steps of: carrying out cyclization in protonic acid including trifloromethanesulfonic acid by taking 3-(2-(4- chlorophenoxyl)-phenyl-4-hydroxyl-1-methyl-1H-pyrrole-2(5H)-ketone (compound 1) or 3-(5-chlorine-2-phenoxyl phenyl)-1-methyl-1H-pyrrole-2(4H)-ketone (compound 4) as a raw material to generate key intermediate compounds 2 and 4 of asenapine; and carrying out reduction reaction to obtain asenapine. The invention has the advantages of novel process route, high reaction yield and low production cost, and has greater application value and social economic effect.

The invention relates to a synthesis method of palmitoyl amino acid sodium in the surfactant field, in particular relates to a method for preparing palmitoyl amino acid sodium by using palmitoyl chloride synthesized by a phosgene method. The synthesis method comprises the following steps: by taking palmitic acid and phosgene as raw materials, preparing palmitoyl chloride through reaction in the presence of an organic amide catalyst; dropwise adding palmitoyl chloride in an amino acid alkaline solution to obtain palmitoyl amino acid through reaction; and dissolving obtained palmitoyl amino acid with ethanol and adding the ethanol solution of sodium hydroxide to finally obtain palmitoyl amino acid sodium. In the synthesis method, a lot of phosphorus-containing wastewater is not produced even though phosphorus trichloride is used as a chlorination agent; sulfur dioxide generated by a thionyl chloride method can heavily pollute the environment; and the synthesis method reasonable in process, high in reaction yield and good in product quality, and the product does not contain residual phosphorus and sulfur and can be widely used in high-end anti-aging cosmetics.

The invention relates to a method for extracting athomin with mustard seeds as the raw material. The method comprises the following steps: taking mustard seeds in brassica in cruciferae as the processing raw material, soaking the raw material in water after being crushed, and then rapidly and effectively obtaining crude product of athomin by a subcritical water extraction method. Because the subcritical water extraction technology is a novel environment-friendly extraction technology not using or rarely using organic solvent, when being in the subcritical state, water has certain dissolving capacity to semi-polar and non-polar organisms, the polarity, the surface tension and the viscosity of water can be changed by controlling the temperature and the pressure of subcritical water, so that the dissolving capacity of the subcritical water to the organisms can be greatly imoroved, therefore, the extraction efficiency is greatly improved, and the content of allyl isothiocyanate product in athomin is high. Compared with the prior art, the method has the advantages of simple technological line, reasonable technological condition, simple and safe reaction and operation, short reaction time, low solvent loss, low technological cost, and high implementation value and social and economic benefit.

The invention belongs to the field of chemical synthesis of medicines, and particularly relates to a preparation method of trelagliptin. A synthesis path of the trelagliptin is shown in the specification. The trelagliptin which is protected by Boc is synthesized by (R)-3-Boc-aminopiperidines, the trelagliptin is obtained through hydrolysis deprotection, by-products produced by reaction on amidogen can be avoided, the synthesis path is novel, technological conditions are reasonable, the type and the content of impurities in the trelagliptin can be controlled effectively, a technology is easy to operate, and the yield is high. Moreover, the preparation method of the trelagliptin is suitable to be produced industrially and has high application value, high social benefit and high economic benefit.

This invention has offered a chemosynthesis method to AE-activity ester, using ATMAA, dibenzthiazole sulfide, triphenylphosphine as raw materials, in existing of catalyst, after sufficient response of the organic solvent, filter the reaction solution, filter cake is washed and dried to get stated AE-activity ester, join di(trichloromethyl)carbonic acid ester in filtrate, the reaction gets dibenzthiazole and triphenylphosphine, stated benzthiazole sulfide and triphenylphosphine can be recycled after being retrieved. This invention has advanced craft route, rational process conditions, cheap and easy getting raw materials, simple and safe operation.

The invention provides a chemical synthesis method of 4-chloromethyl-5-methyl-1, 3-dioxa cyclopentene-2-ketone, which comprises using 4, 5-dimethyl-1, 3-dioxa cyclopentene-2-ketone as raw material and uses sulfuryl chloride as chlorinating agent to process reflux reaction in organic solvent for 1-3h, evaporating out the solvent, rearranging for 1-4h at 70-100DEG C, and separating the reaction liquor after the rearrangement to obtain the 4-chloromethyl-5-methyl-1, 3-dioxa cyclopentene-2-ketone. The chemical synthesis method has the advantages of reasonable process conditions, reliable and safe production, high reaction total yield, low production cost, little discharge of three wastes and significant pratical, social and economic benefits.

The invention belongs to the technical field of pharmacochemistry and in particular relates to a preparation method of a posaconazole intermediate. The method comprises four steps of alkylation, reduction, acylation and cross-coupling, so that a target compound (I) is obtained. Compared with the existing synthetic method, the synthetic method provided by the invention has the characteristics of low price and easiness in obtainment of raw materials, simple and convenient technology, high yield and the like.

The invention discloses a chemical synthetic method for 6, 8-ethyl octylate chloride. The method comprises the steps as follows that: 6-hydroxyl-8-ethyl octylate chloride is dissolved in N, N-dimethylformamide; solution which is dissolved with organic solution of double (trichloride trichloromethyl)-carbonic acid ester is dropped in when in mixing under cold water bath condition; the solution is gradually warmed to 50 to 90 DEG C for reacting for 2 to 8 hours after dropping; and the reaction solution is disposed into 6, 8-ethyl octylate chloride after finishing the reaction. As the invention replaces sulphoxides chloride with double (trichloride trichloromethyl)-carbonic acid ester, the invention produces environment friendly Vilsmeier agent which needs not to be separated in the reaction, and the Vilsmeier agent directly reacts with 6-hydroxyl-8-ethyl octylate chloride to produce 6, 8-ethyl octylate chloride. Besides, the invention has the advantages of advanced technique, rational technological condition, simple and safe operation, high reaction yield, low production cost, low three-waste emission and great implementation value and social and economic efficiency.

The invention discloses a chemical synthesis method for S-(4-tolyl)benzene sulfonate which is shown as a formula (I). According to the method, sodium benzene sulphinate which is shown as a formula (II) and bis(4-tolyl)disulfide which is shown as a formula (III) are used as raw materials; and the S-(4-tolyl)benzene sulfonate is obtained by the steps of fully reacting the sodium benzene sulphinate and the bis(4-tolyl)disulfide in an organic solvent at the temperature of between -40 and 120 DEG C under the action of N-halogenate succinimide, and treating a reaction solution. The process is reasonable, reaction conditions are mild, reaction yield is high, production cost is low, three wastes (waste water, waste gas and residues) are few, and the method has great implementation value and social and economic benefit.

The invention provides a synthesis method of 1,4-butanediamine, which comprises the steps of: (a) dissolving the 1,4-dibromobutyl amine represented by formula (1) in a solvent A, adding the phthalimide potassium represented by formula (2), reacting while stirring at a reflux temperature, filtering reaction liquid, washing by using distilled water to obtain the 1,4-diphthalimide butane representedby formula (3); (b) adding the 1,4-diphthalimide butane obtained in the step (1) and 40% methylamine water solution to a solvent B, heating until solids are dissolved completely, stirring and reacting for 0.5-4 hours at the reflux temperature to obtain reaction products; and (c) filtering the reaction products, post-treating filtrate, distilling the filtrate under normal pressure, and collecting the fractions between 158 DEG C and 160 DEG C to obtain the 1,4-butanediamine. The invention has simple and convenient technological conditions, cheap raw materials, mild reaction conditions, easy control and convenient industrial production.

The invention provides an experimental machine for testing extrusion properties of rubber. The experimental machine for testing extrusion properties of rubber comprises a machine head, a machine body, a transmission mechanism, screws, a temperature control device and a control system. The control system comprises temperature thermocouples arranged on the machine body. The experimental machine for testing extrusion properties of rubber is characterized in that the screws have at least two helical structures; the tails of the screws are removably connected to a main transmission shaft of the transmission mechanism; and the control system also comprises an infrared temperature and speed detection device arranged on a rubber outlet of the machine head, and a torque sensing device arranged on an output shaft of a motor. The experimental machine for testing extrusion properties of rubber can realize comprehensive testing of extrusion performances of rubber prepared according to different formulas, provides reasonable and accurate technical conditions for actual production, improves the quality of rubber materials and rubber products, reduces energy consumption, and provides the basis for designing of various rubber extruders. The temperature control device has a simple structure, is convenient for control, and reduces a loss and a cost.

The present invention discloses a fagopyrum tataricum tea processing method which comprises the following steps: taking fagopyrum tataricum and removing impurities; soaking the fagopyrum tataricum; steaming and boiling the soaked fagopyrum tataricum with controlled temperatures; oven-drying the steamed and boiled fagopyrum tataricum and controlling the water content at 40-50%; decorticating the oven-dried fagopyrum tataricum, removing the fagopyrum tataricum shells, and retaining the fagopyrum tataricum cores to obtain the fagopyrum tataricum rice; oven-drying the fagopyrum tataricum rice until the water content is less than 20%; and frying the dried fagopyrum tataricum rice with controlled temperatures to obtain the finished products. The fagopyrum tataricum tea processing method can improve the rutin content, wheat flavor and mouthfeel of the fagopyrum tataricum tea finished products.

The invention relates to a preparation method of ethyl 6,8-dichlorocaprylate, belonging to the technical field of preparation of organic compound intermediates. The preparation method comprises the steps of reacting ethyl 6-hydroxy-8-chlorocaprylate with a chlorination agent in an organic solvent by taking N,N-dimethylbenzylamine as an acid-binding agent, controlling the reaction temperature, maintaining the temperature after the reaction is finished, and controlling the temperature maintaining temperature and the temperature maintaining time to obtain reaction liquid, adding water for layering to obtain an organic phase at an upper layer, carrying out reduced pressure rectification to obtain ethyl 6,8-dichlorocaprylate, adding alkali to a lower layer to regulate pH for layering, and carrying out dehydration on the upper layer by virtue of anhydrous sodium sulphate so as to obtain N,N-dimethylbenzylamine, and recycling. By virtue of the preparation method, the chlorination capacity is improved, the yield reaches about 95%, the cycle use is realized, the discharging of wastewater is reduced, the process route is advanced, the process conditions are reasonable, the operation is simple and safe, the reaction yield is high, the production cost is relatively low, and three wastes are little.

The invention discloses a green synthesis method for ibuprofen piconol and a medicinal preparation method thereof and provides a formula process of and a green chemical synthesis method of a medicinal compound, in particular the method for preparing ibuprofen piconol, a medicinal composition prepared by using ibuprofen piconol as an active ingredient, and a new formula of an externally-applied preparation for diminishing inflammation, relieving pain and treating infectious diseases. Compared with the prior art, the method has the advantages that: the technical route is advanced, the technical conditions are reasonable, the use of halogenating agents such as thionyl chloride which produce lots of toxic and harmful gases is avoided, a reactions are replaced by one reaction, the operation is simple, convenient and safe, the reaction yield is high, the reaction conditions are easy to control, the solvent and a dehydration condensation agent can be recycled and reused, the problems of trouble of treatment after a reaction process, serious waste gas, waste water and waste residue pollution and the like in the conventional process are solved from the source, environment pollution is avoided, little waste gas, waste water and water residue are produced, and high implementation value and great social and economic benefit are realized.

A process for chemically synthesizing 3,4-dichlorobenzene isocyanate includes such steps as proportionally mixing 3,4-dichlorophenylamine, catalyst and organic solvent to reactor, stirring, dripping the solution of bicarbonate in organic solvent into the solution, reacting at 20-180 deg.C for 3-10 hr, vacuum distilling to recover organic solvent, collecting fraction, cooling and solidifying. Its advantages are high output rate, low cost and less corrosion to equipment.

A technology for preparing the canned red beam includes such steps as choosing raw red bean, washing, immersing, pre-boiling with high-temp steam, disinfecting empty cans by hot water at 82 deg.C or higher temp, filling the pre-boiled red bean in said cans, filling soup at 75 deg.C or higher temp, adding less starch, vacuum sealing, sterilizing at 121 deg.C for 10-60 min, cooling and packing.

The invention relates to a p-chloroaniline isocyanate preparation method comprising the following steps: (1) p-chloroaniline hydrochloride is synthesized, wherein p-chloroaniline is adopted as a raw material and is subjected to a reaction with hydrochloric acid in an organic solvent, such that p-chloroaniline hydrochloride is synthesized; (2) p-chloroaniline isocyanate is synthesized, wherein p-chloroaniline hydrochloride and triphosgene are adopted as raw material, and p-chloroaniline isocyanate is synthesized in an organic solvent. The method provided by the invention has the advantages of advanced process route, reasonable process conditions, and high reaction yield. The materials used in production are not highly excessive; solvent dose in each step is low; and the solvent can be directly used without treatment. An intermediate is not needed to be dried, and can be directly used in the next step of reaction. Three-waste amount is low, and the waste is easy to treat. Therefore, the method has good implementation value and social benefit.

The invention discloses a method for preparing lenalidomide (3-(7-amino-3-oxo-1H-isoindazole-2-yl) piperidine-2,6-diketone). The method comprises the steps of: intramolecular cyclization, deprotection, phase-transfer catalytic reaction, catalytic hydrogenation, alkalization and the like. The technology is novel in path, short in step, high in reaction yield, and low in production cost, and has large implementation value and social and economic benefits.

The invention provides a method of recovering a phosphate radical and a sulfate radical from iron phosphate production wastewater. The method particularly comprises the steps of: (1) adding Ca(OH)2 into an iron phosphate mother solution for reaction to form first sediment residue and first sediment liquid, (2) adding an ammonia-containing solution into the first sediment liquid for reaction to form second sediment residue and second sediment liquid, (3) mixing the first sediment residue and the second sediment residue to form phosphorus containing gypsum, and adding the phosphorus containing gypsum into the iron phosphate mother solution for reaction to form conversion filtrate and calcium sulfate, (4) allowing the conversion filtrate to flow back to the step (1), stopping adding the ironphosphate mother solution, repeating the steps (1), (2) and (3), and (5) mixing the second sediment liquid and acid liquid to form a neutralization regulating solution, and performing reverse osmosis,evaporation and crystallization on the neutralization regulating solution to form an ammonium sulfate solid and a monoammonium phosphate solid. The method can achieve complete separation and thoroughrecovery of the phosphate radical and the sulfate radical in the wastewater, and a phosphate radical product and a sulfate radical product are higher in purity.

The invention discloses a method for synthesizing an aryl monofluoromethylthio compound from a Bunte salt. With a phenylboronic acid derivative and S-(monofluoromethyl) sodium thiosulfate in the Buntesalt as raw materials, copper iodide as a catalyst, 1,10-phenanthroline as a ligand, potassium carbonate as alkali and methanol as a solvent, a reaction is fully carried out at the reaction temperature of 80-90 DEG C. After the reaction is finished, a reaction solution is separated and purified to obtain the aryl monofluoromethylthio compound. The method is reasonable in process condition and easy and safe to operate; the use of thiophenol and other substrates with unpleasant smell is avoided, less waste gas, waste water and industrial residue are generated, and the method is environmentallyfriendly; the reagent is simple in synthesis route and is an odorless solid, treatment is convenient, and the method is a new approach to synthesizing the aryl monofluoromethylthio compound.

The invention relates to an impeller hot pressing manufacturing method which includes the following steps: step 1, cleaning up impeller dies and coating release agent on the dies; step 2, installing the lower die, a charging barrel and a mandril and aligning the inserts; step 3, weighing the materials according to consumption quota and pouring the materials into the lower die; step 4, installing the upper die and putting the dies onto a press to be closed; step 5, exhausting the air of the dies; step 6, gradually pressing until reaching the prepressing pressure; step 7, after prepressing, heating the dies; step 8, after heating, putting the dies onto the press to be extruded until reaching the dwell pressure; step 9, dwelling under pressure and solidifying, and after that taking off the dies; step 10, demoulding; and step 11, cleaning up the dies and furnishing and cleaning up the impeller. Repeated experiments show that the method has the characteristics of high efficiency, low cost and reasonable technical condition and the piece manufactured through the method is of high quality.

The invention discloses a chemical synthesis method of octadecyl isocyanate; wherein, the method adopts octadecyl amine and bi(trichloromethyl) carbonate as raw materials, organic solvents are used for dissolving the octadecyl amine solution to be slowly dropped into the solution of the bi(trichloromethyl) carbonate dissolved by the same organic solvent, the temperature of a reaction system is kept from 0 to 5 DEG C, and after the dropping is finished, the solution is stirred for 0.5 hour to 5 hours at room temperature, then the temperature is increased to 35 to 150 DEG C and the solution is reacted at the temperature of 35 to 150 DEG C for 0.5 hour to 10 hours and then the octadecyl isocyanate is obtained after the reaction solution is post treated. The chemical synthesis method is advanced in technical route, reasonable in technical condition and eliminates potential safety hazard from headstream; the used raw materials are cheap and easy to be obtained; the use of highly toxic gas phosgene controlled internationally is abolished and the problems of big potential safety hazard and severe three wastes, etc. of traditional technologies are eliminated; the chemical synthesis method is simple and safe in operation, high in reaction yield, low in production cost and basically has no three wastes and has greater implement value and social economic benefits.

The present invention provides the reaction process of di(trichloromethyl) carbonate and 2, 2'-dithio diphenyl formic acid at 20-150 deg.c inside organic solvent under the action of organic amine catalyst to prepare 2, 2'-dithio diphenyl formyl chloride. The chemical synthesis process eliminates unsafe hidden trouble and environmental pollution radically, and has the advantages of cheap material, high safety and reliability, high reaction yield, low production cost and no waste generated.

The invention relates to a synthesis method for co-producing p-chloroaniline and p-chlorophenol isocyanate. The method comprises the following steps of: reducing parachloronitrobenzene by using iron powder, separating water, dehydrating, adding a solvent, reacting with a bis(trichloromethyl) carbonate solution, distilling to recover the solvent, and distilling to obtain a p-chlorophenol isocyanate finished product. The method has the advantages that a process is advanced; process conditions are reasonable; the production of p-chloroaniline is organically combined with that of p-chlorophenol isocyanate; the environment pollution and an intoxicating phenomenon which are brought by p-chloroaniline used as an industrial product in the processes of aftertreatment, conveying, carrying and feeding can be avoided; virulent phosgene and diphosgene are avoided during production of p-chlorophenol isocyanate, and production is safe and reliable; the residual bis(trichloromethyl) carbonate is removed by normal-pressure reflux; the improvement on the quality of a product is facilitated; and the method has great implementation value and social and economic benefits.

The invention discloses a method for rapidly printing on the surface of a fabric. The method is characterized by comprising the following steps of: slightly pulling the fabric so as to enable the fabric to be in a tensioning state; preheating the fabric by adopting a thermal roll at 40 DEG C to 60 DEG C; spraying pigment on the surface of a printing roller with patterns, and raising the temperature of the printing roller to 60 EDG C to 80 DEG C by adopting an electric heating manner; rolling the printing roller on the fabric so as to finish the printing, wherein the pressure of the printing roller is 10-15 MPa; and baking at 50 DEG C to 60 DEG C for 1-2 hours. The method has a simple process, and is easy to operate and high in printing efficiency.

The invention discloses a synthesis method of S-substituted-anthranilate thioester derivatives disclosed as Formula (I), which comprises the following steps: sufficiently reacting isatoic anhydride compounds disclosed as Formula (II) and dithioether compounds disclosed as Formula (III) in an inert organic solvent at 0-120 DEG C in the presence of an accelerator and basic compounds; and after the reaction finishes, separating and purifying the reaction solution to obtain the S-substituted-anthranilate thioester derivatives disclosed as Formula (I). The method disclosed by the invention has the advantages of reasonable technological conditions, simple and safe operation, mild reaction conditions, high reaction yield, cheap and accessible raw materials, environment-friendly substrate, low production cost and fewer three wastes.

The invention provides a chemical synthesis method of 4-bromomethyl-5-methyl-1, 3-dioxa cyclopentene-2-ketone, which comprises using 4, 5-dimethyl-1, 3-dioxa cyclopentene-2-ketone as raw material and uses N-bromosuccinimide as bromination agent to be reacted in the presence of initiator and in organic solvent, separating and purifying the reaction liquor after the reaction, to obtain 4-bromomethyl-5-methyl-1, 3-dioxa cyclopentene-2-ketone. The chemical synthesis method of 4-bromomethyl-5-methyl-1, 3-dioxa cyclopentene-2-ketone has the advantages of reasonable process conditions, reliable and safe production, simple operation, little discharge of three wastes and benefit for industrial production.

The invention relates to a chemical synthesis method of 2-hydroxy benzimidazole, which takes o-diaminobenzene and bis (trichloromethyl) carbonate as raw materials. The raw materials are put into organic solvent for react for 1-13h at -10-80 DEG C with the effect of organic alkali, after-treatment is carried out to reaction solution to get the 2- hydroxy benzimidazole. The chemical synthesis method of the 2- hydroxy benzimidazole of the invention has reasonable technical conditions, the used raw materials are cheap and can be obtained easily, the operation is simple and safe, the reaction conditions are mild and the production cost is low with less three wastes, thereby having higher implementation value and social and economic benefits.