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 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.

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 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 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.

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.

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 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.