95results about How to "Advanced process route" patented technology

The invention provides a method for chemically synthesizing iminostilbene which is shown as a formula (I), comprising the following steps that: catalyst is filled on a fixed catalyst bed, the temperature of the catalyst bed is increased to between 400 and 600 DEG C by heating the catalyst bed electrically, iminodibenzyl which is shown as a formula (II) and is pre-heated to be liquated is sent to the fixed catalyst bed through high-pressure water vapour, the flow rate of the water vapour is controlled to between 0.2 and 20l/h by the iminodibenzyl fluid volume, and the material which passes through the fixed catalyst bed is put into a receiving device holding cooling water to produce the mixed fluid which is subject to moisture evaporation to dryness is crystallized again so that the iminostilbene is obtained. The method mainly has the advantages of high reaction yield coefficient up to 93.8 percent, low production, advanced process flow and convenient operation.

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 the field of medicine synthesis, and discloses a preparation method of a Palbociclib intermediate. In the preparation process, 5-bromine-2,4-dichloropyrimidine is used as a starting raw material; through ammoniation substitution reaction, green solvent PEG (polyethylene glycol) promotion palladium catalysis coupled reaction, BTC (triphosgene) promotion cyclization reactionand NBS (N-bromosuccinimide) bromination reaction, a target compound V is finally obtained; through aftertreatment improvement, the HPLC purity of the final product can reach 99 percent or higher. Compared with a traditional process, the preparation method has the main beneficial effects that the reaction conditions are mild; the operation is simple and convenient; the palladium catalyst consumption is low; the yield is high; the cost is low; the three-waste quantity is small; the industrialization is easy; high implementation values and socioeconomic benefits are realized.

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 relates to a technique for recycling aluminum hydroxide from acid washing waste liquor and alkaline washing waste liquor of an aluminum-based material. The technique is characterized by comprising the following steps of: (1) respectively pre-treating the acid washing waste liquor and the alkaline washing waste liquor of the aluminum-based material; (2) mixing and separating the pretreated acid washing and the alkaline washing liquor after being neutralized, discharging the waste water after reaching the standard and directly utilizing a filter cake - aluminum hydroxide as an industrial raw material. According to the technique, not only is a great amount of aluminum-based alkaline washing waste liquid and acid washing waste liquid successfully treated, but also byproducts can be recycled, no secondary pollution occurs, and the technical difficulty both at home and abroad for a long time can be solved. A pilot scale test shows that the technique is reasonable in design and easy to implement and has great social benefit, environmental-protection benefit and economic benefit.

The invention discloses a method for effectively recycling 2,4-dichloro-5-fluoro acetophenone from crystallization mother liquor, which comprises the following steps of: (a) reacting 2,4-dichloro-5-fluoro acetophenone crystallized mother liquor and neopentyl glycol as raw materials in an inert organic solution A under the action of an acidic catalyst A, then removing water continuously produced in the reaction process, and after sufficient reaction, separating and purifying to respectively obtain 2,6-dichloro-3-fluoro acetophenone and 2,4-dichloro-5-fluoro acetophenone ketal; and (b) carrying out the hydrolysis on the 2,4-dichloro-5-fluoro acetophenone ketal and water in an inert organic solution B under the action of an acidic catalyst B, and after sufficient reaction, carrying out aftertreatment to obtain the 2,4-dichloro-5-fluoro acetophenone. The invention has advanced process route, simple operation, mild reaction condition, high recycle rate of the 2,4-dichloro-5-fluoro acetophenone, environment protection and low production cost; and the neopentyl glycol of the auxiliary reagent can be recycled repeatedly, and the solidoid acidic catalyst can be recycled, thereby the invention is suitable for industrialized large-scale production.

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 belongs to the field of medicine and particularly relates to a method for preparing a solifenacin intermediate. After 2-halogenated diphenyl ketone is used for carbonyl protection, n-butyllithium is used for removing bromine, then the formyl group is added; a condensation reaction with nitromethane and catalytic hydrogenation for reduction are carried out, and then acidification is conducted; later, cyclization is carried out, and a solifenacin intermediate compound I is obtained through alkaline hydrolysis after reduction and chiral resolution. The structural formula of the solifenacin intermediate is shown in the description. According to the method for preparing the solifenacin intermediate, the initial raw materials easy to obtain are utilized, and the production cost is reduced. The process route is advanced, the reaction conditions are mild, the reaction yield is high, less three wastes are caused, expensive and toxic reagents do not exist, reaction solvents can be used repeatedly after distillation, industrial production is facilitated, and implementation value and social, economic and environmental protection benefits are high.

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.

Provided is a method for synthesizing carbamazepine. The method comprises the steps that 1 part by weight of iminostilbene and 10 parts by weight of benzene are put into a glass lining reaction vessel of 1,000 L to be dissolved, and the materials react with 0.7 part of triphosgene for 5 h to 6 h at 70 DEG C to 80 DEG C after being dissolved to enable all the materials to react completely; 2/3 of benzene is distilled off through reduced pressure distillation, suction filtration is conducted after cooling is conducted, the materials are put into a drying oven or a drying room to be dried for 3 h to 4 h at 60 DEG C after being filtered, iminostilbene carbonyl chloride is obtained and put into a glass lining reaction vessel of 1,000 L, 15 parts of 95% ethyl alcohol is added, the materials are dissolved in the glass lining reaction vessel, 0.8 part of liquid ammonia is dropwise added, reacting is conducted for 8 h at 50 DEG C to 60 DEG C, heat preservation is conducted for 30 min, all the materials are cooled to room temperature, 1%-3% by weight of activated carbon is added, the temperature is increased to 78 DEG C, decoloration is conducted for 2 h, a mother solution is subjected to hot filtration, residues are discarded, and the mother solution is sent back to the glass lining reaction vessel; 1/2 of ethyl alcohol is distilled off, after cooling is conducted, natural crystallization and suction filtration are conducted, a crystal substance obtained after filtration is conducted is put into the drying oven or drying room to be dried for 3 h to 4 h at 60 DEG C, and the finished carbamazepine product is obtained. The yield ranges from 82% to 90%, and the content ranges from 91.5% to 99.1%.

The invention relates to a method for synthesizing 2-aminothiazoline, which comprises the following steps: firstly, performing chlorinated reaction between ethanolamine and thionyl chloride in an organic solvent to generate 2-chloro-ethylamine hydrochloride; and secondly, performing cyclization reaction between the 2-chloro-ethylamine hydrochloride and thiourea to generate the 2-aminothiazoline. Compared with the prior art, the method does not need introduce hydrogen chloride gas and concentrated hydrochloric acid to synthesize ethanolamine hydrochloride, thereby reducing reaction reagents and the reaction steps; besides, the process route is more advanced, environment-friendly and safer, and the cyclization yield reaches more than 70 percent.

The invention discloses a preparation method for 2-cyano-4'-methylbiphenyl. The invention adopts the following technical scheme: the preparation method comprises the following steps: taking p-chlorotoluene as a raw material for Grignard reaction with magnesium powder in a solvent in the absence of water under nitrogen protection, and coupling a reaction product with chlorobenzonitrile under the catalytic effect of a nickel-manganese composite catalyst to prepare 2-cyano-4'-methylbiphenyl. A Ni (II)/Mn (II) composite catalyst is added into a 2-cyano-4'-methylbiphenyl synthesis reaction system, so that the reaction activity is enhanced and the reaction selectivity is improved; the catalyst is lower in price and easy to recover, so that the postprocessing difficulty is lowered and the production cost is reduced; a recrystallization method is adopted in postprocessing and refining processes, so that the product purity is further improved, a white product is obtained, and the industrialization operation is more convenient.

The invention discloses a green synthesizing method of triphenylchloromethane. The synthesizing method comprises the following steps of: using triphenylmethanol as raw material; reacting the triphenylmethanol with triphosgene in an organic solvent for 0.1-20 hours at a temperature of -20-150 DEG C; after reacting, separating to obtain a crude product; and recrystallizing the crude product to obtain the triphenylchloromethane, wherein the mass ratio of the triphenylchloromethane to the triphosgene is 1:(0.33-2). The synthesizing method has the advantages of reasonable process, high reaction yield, low production cost, less three waste and simple aftertreatment.

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 discloses a chemical synthetic method of 2-imidazole flavanone. The synthetic method comprises the following steps: ethylenediamine and 2 to 20 percent of sodium hydroxide solution are added in a reactor; at the temperature from minus 10 DEG C to 50 DEG C, bi(trichloromethyl) carbonate is slowly dropped into the reactor for 1 to 15 hours; then the mixture reacts for 1 to 20 hours at the temperature from 0 DEG C to 80 DEG C; after the reaction, the reaction solution can be treated to prepare the 2-imidazole flavanone. The chemical synthetic method has high yield (generally above 80 percent) and high purity (generally above 98.0 percent). Thus the chemical synthetic method is an effective synthetic method with reasonable process, low production cost, high yield and less three-waste.

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 of tert-butyl isocyanate. The synthesis method comprises following steps: (1) evenly mixing a proper amount of catalyst and a solvent (90% of the theoretical amount) at a temperature of 90-180 DEG C to obtain a premixed solution, gradually dropwise adding a fed-batch solution into the premixed solution, after addition, maintaining the temperature of reaction solution in a range of 90-180 DEG C, keeping a reflux state, and carrying out reactions for 15 to 25 hours under stirring; and (2) after the reactions (1), delivering the mixed solution to a rotary evaporator, carrying out rotary evaporation, washing, and drying to obtain a tert-butyl isocyanate product. According to the synthesis method, tert-butyl amino formyl chloride directly carries outreactions in an inert solvent to prepare tert-butyl isocyanate; the safety hazard is radically inhibited from the source of the technology, and the preparation method has the advantages of reasonabletechnology, safety, high yield, and low production cost, and does not generate any wastewater, waste gas, or waste solid.

The invention discloses a method for chemically synthesizing 3,5-diio-2-hydroxybenzene formyl chloride. The method comprises the step of: with 3,5-diio-2-hydroxybenzoic acid and di(trichloromethyl) carbonic ester as raw materials, reacting for 1-10 hours at the temperature of 40-150 DEG C in an organic solvent under the action of an organic amine catalyst, and processing reaction liquid to obtain 3,5-diio-2-hydroxybenzene formyl chloride, wherein the charging mol ratio of the 3,5-diio-2-hydroxybenzoic acid to the di(trichloromethyl) carbonic ester is 1: (0.34-2.0), the charging mol ratio of the 3,5-diio-2-hydroxybenzoic acid to the organic amine is 1: (0.01-1.0), and the mass ratio of the organic solvent to the 3,5-diio-2-hydroxybenzene formyl chloride is (5-20): 1. The method disclosed by the invention has the advantages of available raw materials, low cost, simplicity and safety in operation, environmental friendliness and higher product yield and purity and has greater application value and good social and economical benefits.