66 results about "Propargyl alcohol" patented technology

The invention relates to the technical field of synthesis of propargyl chloride, in particular to a synthesis method of propargyl chloride. When 3-chloropropyne is synthesized by a conventional method, the yield is difficult to reach 90% or above. In order to solve the technical problems, the invention provides the synthesis method of the propargyl chloride, and propargyl alcohol and hydrogen chloride are subjected to substitution reaction in an organic solvent to generate the 3-propargyl chloride under the action of a closed reactor and a catalyst. According to the method for synthesizing the 3-chloropropyne, the yield of the 3-chloropropyne is larger than or equal to 90%, and the generation amount of by-products is smaller than 5%. The by-product hydrogen chloride is directly used as a synthesis raw material, so that the raw material cost is remarkably reduced. The method is mild in reaction condition, low in equipment investment and suitable for industrial amplification.

The invention relates to a process for the production of an organic layer comprising regions with different electronic properties. The process is based on the use of dihydroanthracene, dihydrobenzene, benzol or fluorene precursors functionalised with at least one substituted propargyl alcohol. By subjecting these precursors to a reduction / re-aromatisation reaction and / or to a retro-Favorskii reaction one obtains small organic molecules or polymers having different electronic properties, due to the specific chemical composition generated by the different chemical reactions in which the precursors are involved. Therefore, starting from the same precursor and subjecting it alternatively to the two specified reactions, one obtains products with different electronic properties. i.e. molecules characterised by high energy levels of the highest occupied molecular orbital (HOMO), which have at least one aromatic ring substituted with at least one ethynyl group, and molecules characterised by lower energy levels of the lowest unoccupied molecular orbital (LUMO), which have at least one carbonyl functionality, preferably at least one quinone ring or at least one phenyl with at least one carbonyl functionality. The reactions are carried out in such a way that the final products are incorporated into a single organic layer.

An inhibition corrosion package for use with an acidic composition, where the package includes a terpene component; a propargyl alcohol or derivative thereof; optionally, a tall oil fatty acid; at least one amphoteric surfactant; and a solvent. Also disclosed are acidic compositions combining the corrosion inhibition package for use in various industrial operations including, but not limited to, oil and gas operations. Also disclosed are methods of using such compositions.

The invention discloses a preparation method of a cyanoborate lithium salt derivative, which comprises the following steps: 1, mixing an alcohol compound, a lithium source compound, a boron source compound and trimethylsilyl cyanide in a polar organic solvent, and filtering after complete reaction to obtain a cyanoborate crude product filtrate; the alcohol compound is selected from one of 2, 2, 2-trifluoroethanol, 2, 2-difluoroethanol, 2-fluoroethanol, 3-hydroxypropionitrile, allyl alcohol and propargyl alcohol; the lithium source compound is selected from one of lithium carbonate and lithium hydroxide; the boron source compound is selected from one of boric acid, diboron trioxide and boron tribromide; the reaction temperature is controlled to be 0-120 DEG C; and 2, adding an inert organic solvent into the cyanoborate crude product filtrate for crystallization, and performing vacuum drying to obtain a finished product of the cyanoborate lithium salt. The method has the advantages of high yield and purity, simple process, convenience in operation and low cost, and is extremely suitable for industrial production.

The present application relates to the technical field of fine chemical product synthesis, and in particular to a synthesis method of 3-chloropropynyl co-production of p-chlorobenzaldehyde, which comprises the following steps: mixing propargyl alcohol, a solvent, an ionic liquid catalyst, a cocatalyst DMF and a polymerization inhibitor p-tert-butyl catechol, heating and slowly adding p-chlorobenzylidene dichloride dropwise into the mixture, collecting the generated 3-chloropropynyl crude product at the tail gas outlet, cooling after the reaction is completed, and sequentially reducing pressure rectification of 3-chloropropynyl, the remaining propargyl alcohol and the solvent, and p-chlorobenzaldehyde product through a rectification tower. The present application solves the problems of using toxic and hazardous chemicals chlorinating agent in the production of existing 3-chloropropynyl, and generating a large amount of toxic waste acid gas or low-value byproducts, and the problem of low utilization rate of chlorine atom in the existing direct hydrolysis method of p-chlorobenzaldehyde, and reduces environmental pollution.

The invention discloses a continuous flow preparation method of polysubstituted propargyl alcohol, which uses a microtube continuous flow reaction device and comprises the following specific steps: simultaneously conveying acetylene gas or terminal alkyne compound and an organic alkali solution into a mixer for premixing; simultaneously conveying the keto-carbonyl substrate and the flowing-out reaction liquid to a reactor to carry out an alkyne hydrogenation reaction; and carrying out gas-liquid separation on the outflowing reaction liquid, and rectifying in a rectifying tower to obtain a target propargyl alcohol product. According to the method for continuously preparing the polysubstituted propargyl alcohol by using the continuous flow reaction system, full mixing of reaction materials of each reaction unit and accurate control of the reaction can be realized by regulating and controlling pipeline parameters, the automation degree is greatly improved, the manual operation is reduced, the energy consumption cost is reduced, and the method is suitable for industrial production.

The application discloses a catalytic synthesis method of chiral polysubstituted hydrogenated quinoline compounds, and belongs to the field of organic synthesis. The application comprises the following steps: at 0-40 DEG C, alcohol or halogenated alkane is used as a solvent, a copper metal catalyst and a chiral ligand are added, and reaction is carried out under nitrogen protection for 0.5-2 hours; the temperature is lowered to-60-0 DEG C; then, o-aminophenyl nitrone, propargyl alcohol ester and alkali are sequentially added; and reaction is carried out for 6-48 hours, so as to obtain a chiral polysubstituted hydrogenated quinoline compound shown in formula 1 or 2. The application realizes, for the first time, synthesis of chiral polysubstituted hydrogenated quinoline compounds by using o-aminophenyl nitrone and propargyl alcohol ester as reactants, and by using a cheap copper metal catalyst and a chiral ligand, the method is simple in operation, low in cost, and has excellent enantioselectivity and diastereoselectivity.

The present invention relates to a Zr-based Cr / P-free composition for treating a metal surface, comprising: (A) a source of hexafluorozirconate ions; (B) Zn cations; (C) Mg cations; and (D) at least one corrosion inhibitor selected from the group consisting of a propargyl alcohol alkoxy compound and its derivatives, a thiodiglycol ethoxylate and its derivatives, and combinations thereof; wherein the pH value of the composition is in the range of from 3.5 to 6.5, and the concentration of the component (A) calculated on the basis of Zr element is higher than 5 ppm, based on the total weight of the Zr-based Cr / P-free composition. The present invention also relates to a process for treating a metal surface with the composition, and a substrate containing a metal surface treated by the process.

The invention discloses a preparation method of tris (propargyl) phosphorus oxide, and belongs to the technical field of battery electrolyte additives, and the preparation method specifically comprises the following steps: S1, carrying out low-temperature in-situ Grignard exchange and addition reaction, the method comprises the following steps: carrying out in-situ Grignard exchange and addition reaction on phosphorus trichloride, an alkyl lithium reagent and propargyl alcohol in an organic solvent to generate an intermediate tris (propargyl) phosphorous acid; s2, oxidation reaction: adding an oxidizing agent into the reaction system obtained in the step S1, and carrying out oxidation reaction to obtain tris (propargyl) phosphorus oxide; according to the method, the technical bottleneck of preparing the phosphorus-containing alkyne additive by a traditional fractional step method is broken through, a one-pot low-temperature synchronous dropwise adding in-situ reaction process is initiated, and efficient and high-selectivity synthesis of tris (propargyl) phosphorus oxide is realized.

The invention discloses a method for synthesizing chiral morpholine from propargyl alcohol ester. Chiral morpholine is an important drug molecular skeleton and is widely applied to the aspects of analgesia, anesthesia, tumor resistance, heart treatment and the like as a drug active ingredient, but an efficient synthesis method is lacked. According to the method disclosed by the invention, under the regulation and control of arylboronic acid and a specific chiral ligand, propargyl alcohol ester and an affinity reagent react to obtain optically pure (87-97% ee) morpholine. The method has the characteristics that the catalyst and the ligand are wide in source, and the substrate is cheap and easy to obtain; the chiral morpholine has excellent enantioselectivity and good functional group compatibility, can be suitable for structural modification of bioactive molecules and intermediates, and is a simple and efficient asymmetric catalysis strategy for synthesizing chiral morpholine.

The invention relates to the technical field of organic chemical synthesis, in particular to a carbazole axially chiral tetra-substituted allene derivative which is a compound containing a structure shown in the formula (III), R1 is connected with a benzene ring, and R1, R2 and R3 are independently selected from H, alkyl, halogen, silicon, alkenyl, alkynyl, aryl, acyl, sulfonyl, heteroaryl and benzyl. Compared with the prior art, the carbazole axially chiral tetra-substituted allene derivative is obtained by combining the carbazole compound and the propargyl alcohol compound in an addition manner, and the carbazole axially chiral tetra-substituted allene derivative has an allene skeleton and a carbazole active fragment at the same time; the compound can be used as a potential skeleton for developing novel antibacterial and antitumor drugs.

This invention relates to the field of lithium battery electrolyte technology, specifically a method for synthesizing tripropynyl phosphate, comprising the following steps: 1) In a dry reaction vessel, an organic solvent is added, and phosphorus oxychloride is dissolved in the organic solvent, and stored under an inert atmosphere at low temperature; 2) A mixture of propynyl alcohol and triethylamine is slowly added dropwise, and the reaction is continuously stirred while maintaining a low temperature; 3) The mixture is slowly added dropwise, and the reaction is stirred after the temperature is raised to room temperature; 4) The mixture is slowly added to the reaction vessel, and the reaction is stirred after the temperature is raised to room temperature; 5) The triethylamine hydrochloride is removed by filtration, and the filtrate is distilled under reduced pressure to obtain a crude product, which is then purified by reduced pressure distillation or column chromatography. This invention effectively solves the problems of violent exothermic reactions, numerous side reactions, harsh reaction conditions, and difficulties in post-processing and purification of the product in existing synthesis methods by rationally designing reaction steps and precisely controlling reaction conditions and molar ratios.

This invention relates to the field of organic synthesis technology, and more particularly to a method for preparing sulfone-substituted indene compounds. The method involves mixing a propargyl alcohol compound, a sodium sulfinate compound, an acid promoter, and a solvent, and carrying out a tandem sulfonation-cyclization reaction to obtain the sulfone-substituted indene compound. This method has the advantages of readily available raw materials, no catalyst required, ease of operation, and being green and efficient, showing good prospects for industrial application.

The application discloses a lubricating coating for high-temperature fasteners and a preparation method and application thereof. The lubricating coating is prepared by using inorganic phosphate as a binder, nano boron nitride, silver powder, molybdenum disulfide and tungsten disulfide as composite lubricants, antimony trioxide as an antioxidant, nano silicon dioxide as a phosphate binder reinforcing agent, water and anhydrous ethanol as a dispersion medium, and propargyl alcohol as a corrosion inhibitor. The coating is immersed or sprayed on the fastener, and a coating is formed after a certain curing condition. The coating has good adhesion, flexibility and impact resistance, and has no corrosion defects such as pitting, cracking and bubbling after an acetate salt spray test (AASS) for 240 hours. According to the locking torque test in accordance with HB 7687-2001, the locking torque requirement is met after 15 cycles at room temperature and 5 times of warm loading and then air cooling to room temperature. The application has a good application prospect in the field of high-temperature fastener coatings.

The application discloses a kind of water-based polyurethane coating and preparation method thereof, it is related to paint technical field.The water-based polyurethane coating prepared in the application includes component A and component B, component A includes modified polyurethane dispersion, wetting agent, defoaming agent, thickening agent, stabilizer;Component B includes modified silica, dispersant, wetting agent;The modified polyurethane dispersion is prepared by isofuroxone diisocyanate, phosphorus-containing dihydric alcohol, propargyl alcohol, dimethylol butyric acid reaction;The modified silica is the silica that is wrapped by chitosan, after aldehyde group is formed, and functional monomer grafting, and the gamma-seleno butyrolactone obtained by reaction again.The water-based polyurethane coating prepared in the application has good flame-retardant, antibacterial, anti-aging and self-repairing performance.

The invention provides a zinc-based MOF material catalyst and a preparation method thereof, and the zinc-based MOF material catalyst is mainly prepared from the following raw materials: an organic monomer a, a zinc salt, an organic monomer b, a solvent and a metal salt, the organic monomer a is selected from at least one of imidazole nitrogen heterocyclic ligands with carboxylic acid functional groups; the organic monomer b is selected from at least one of difunctional ligands containing amino groups and carboxylic acid groups. The zinc-based MOF material has better carbon dioxide adsorption performance through the synergistic effect of the metal salt and the ligand, can efficiently catalyze the cycloaddition reaction of carbon dioxide and propargyl alcohol as a catalyst under mild conditions, and solves the problems of yield and purity of reaction products.

The application discloses a method for preparing aromatic benzyl propargyl ketone by light induction and biological application, belongs to the technical field of organic synthesis and biological medicine, and converts aromatic benzyl propargyl alcohol into aromatic benzyl propargyl ketone under the condition of light induction; the change of the functional group before and after light induction is that the hydroxyl alkyne without reaction activity is converted into the carbonyl alkyne with click reaction activity, fluorescence enhancement can be realized, and the method can be used for imaging and tracing; and the aromatic benzyl propargyl ketone can react with a compound containing an amino group or a biological macromolecule to realize the killing of tumor cells. The method uses light as a starting switch, the reaction condition is simple, controllability is good, no additional catalyst is needed, and the method is easy to mass-produce, so the method has wide application prospects in polypeptide or protein labeling, anti-tumor and the like.

The utility model relates to the field of chemical separation, in particular to a separation and purification system for synthesizing propargyl alcohol, which comprises a gas mixing device, an acetylene gas pressurizing device, an ethynylation reaction device, a gas-liquid separator, a butynediol separation tower, a formaldehyde recovery tower, a methanol separation tower, a propargyl alcohol product tower and a chromatography device which are connected in sequence. The system disclosed by the utility model can improve the selectivity of propargyl alcohol in the production process of butynediol under the condition of ensuring the safety of high-pressure acetylene, and effectively realize the separation of propargyl alcohol, so that the supply capacity of propargyl alcohol in the market is obviously improved. The device disclosed by the utility model not only improves the yield of the byproduct propargyl alcohol in BYD production, but also separates and extracts important chemical raw materials such as 1, 4 butynediol.

The invention discloses a method for synthesizing phenyl propargyl fluorine compounds from sulfur hexafluoride, and belongs to the technical field of organic intermediate synthesis. The synthesis method comprises the following steps: placing a phenyl propargyl alcohol compound, a photocatalyst, a base, and a solvent in a reaction vessel, filling with sulfur hexafluoride gas, and reacting under light conditions to obtain a phenyl propargyl fluorine compound. Beneficial effect: Compared with other methods for synthesizing propargyl fluorine compounds, the reaction conditions of the present invention are mild, the reaction raw materials used (including propargyl alcohol and N,N-diisopropylethylamine) are cheap and easy to obtain, and SF6 gas can be well utilized with lower energy under blue light irradiation. The reaction has the characteristics of low cost, low energy consumption and environmental friendliness.

The present invention provides a kind of thermosensitive cell microcarrier and preparation method thereof, and the method for culturing cells. The preparation method provided by the present invention, using glass microspheres as basic materials to carry out surface hydroxylation, then aminosilane coupling agent is used to carry out amino modification, then the N-carboxylic acid anhydride (NCA) of glutamic acid modified by propargyl alcohol is polymerized on the surface of glass microspheres, and finally click chemistry reaction is carried out with azido oligoethylene glycol to obtain a surface-covered thermosensitive polymer glass microsphere with good cell compatibility. The thermosensitive cell microcarrier prepared by the present invention has extremely low cytotoxicity and good biosafety; moreover, it has thermosensitive performance, can achieve efficient cell adhesion and detachment, and effectively detaches cells in a low temperature environment; when it is used as a carrier to culture cells, three-dimensional space is provided to cell growth, and compared with a two-dimensional plane, cell amplification can be achieved, the cost of cell culture is reduced, and the effect of protecting cell surface proteins is possessed.

The application provides a base-promoted system for synthesizing alkenyl borate from propargyl alcohol compounds, which comprises propargyl alcohol compounds, a diboron reagent, a base and a solvent. The application also provides an application of the base-promoted system, which is used for synthesizing alkenyl borate from propargyl alcohol compounds through a borohydride reaction. The method is as follows: under the action of a base and a solvent, a borohydride reaction of propargyl alcohol compounds is promoted by using a diboron reagent as a boron source, so as to synthesize alkenyl borate in a trans stereospecific and beta-regioselective manner. In the reaction system, the trans stereospecific and beta-regioselectivity of the borohydride addition of propargyl alcohol compounds are realized, and a transition metal catalyst is not needed, and the system has the advantages of wide substrate application range, high conversion rate and mild reaction conditions.

An isatin-based indolodihydrochromene anti-tumor compound and its synthesis method. The chemical structural formula of the compound is shown in Formula 3. The synthesis method is as follows: The isatin-derived propargyl alcohol and 2-indolylphenol derivative are added to ethyl acetate as reaction raw materials, and under the catalysis of p-toluenesulfonic acid, the reaction is stirred at 25 °C for 8-12 hours. The reaction is tracked by TLC until it is complete, and then filtered, concentrated, and purified to obtain the product. The isatin-based indolodihydrochromene compounds synthesized in the present invention, through bioactivity tests, show that these derivatives have high sensitivity and strong cytotoxic activity against human nasopharyngeal carcinoma cells HONE-1. The reaction conditions of the present invention are relatively conventional, the reaction process is mild, simple, and low-cost, suitable for large-scale industrial production, and broaden the scope of application of this method; the present invention uses a relatively large variety of substrates as reactants, obtaining products with diverse structures and high yields.

The invention discloses a process for preparing 3-chloropropyne through concerted catalysis of phosphine ligand-transition metal in the technical field of organic synthesis. The process realizes efficient synthesis through specific steps: firstly, mixing a porous nitrogen-doped carbon-loaded phosphine ligand-metal nano composite material, palladium chloride and triethylamine under the protection of nitrogen to form a catalytic system; dissolving propargyl alcohol and N-chlorosuccinimide in anhydrous tetrahydrofuran, and mixing in an ice bath to obtain a pre-reaction mixture; then adding the pre-reaction mixture into a catalytic system, stirring and reacting at a specific temperature under the protection of nitrogen, and monitoring the progress through thin layer chromatography in the reaction; and after the reaction is finished, filtering and separating the catalyst, evaporating filtrate under reduced pressure to remove the solvent, and purifying by column chromatography to obtain a target product. The process is high in catalytic efficiency, good in selectivity, high in product yield and environment-friendly.

The utility model belongs to the technical field of 1, 4-butenediol processing, and particularly relates to a device for separating inorganic salt in 1, 4-butenediol, which is connected with a hydrogenated liquid storage tank through a BED hydrogenation section, is sent to a distillation kettle through a hydrogenated liquid feeding pump, enters a dehydration kettle after gas phase condensation of the distillation kettle, and is sent to an incinerator for incineration. A BED crude product obtained after dehydration of the dehydration kettle is sent to a crude product storage tank and is sent to a rectification system through a BED feeding pump to be rectified to obtain a final qualified product, and dehydration kettle liquid is sent to an incinerator to be incinerated. According to the present invention, with the process, the inorganic salt in the crude product is substantially reduced, the problem of frequent blockage of the dehydration kettle discharge pipeline is solved, and the qualified 1, 4-butylene glycol product can be successfully produced from the high-salt-content raw material 1, 4-butynediol (propargyl alcohol by-product).

This application provides a method for preparing methylcarboxylic acid-2-propynyl ester, comprising the following steps: (1) mixing dimethyl carbonate and propargyl alcohol, adding a first alkaline catalyst, stirring and heating to a temperature of 90-105°C, and distilling out methanol by reactive distillation to obtain a first component; (2) performing solid-liquid separation on the first component to obtain a first liquid, and performing vacuum distillation on the first liquid to remove propargyl alcohol and dimethyl carbonate to obtain methylcarboxylic acid-2-propynyl ester and residue; (3) performing vacuum distillation on the residue, replenishing dimethyl carbonate and the second alkaline catalyst with the distillate for reaction, and reusing the reaction liquid in step (2). This application uses the transesterification reaction of propargyl alcohol and dimethyl carbonate to synthesize methylcarboxylic acid-2-propynyl ester, which has high safety, low overall reaction temperature, fewer by-products and waste, and high yield.

The invention belongs to the field of new materials, and discloses a preparation method of 1-propylene-1, 3-sultone, which comprises the following steps: step 1, addition reaction: using propargyl alcohol and alkali metal sulfite and / or alkali metal hydrosulfite as raw materials, and carrying out addition reaction in the presence of a catalyst and a free radical initiator to obtain an addition product; step 2, acidification reaction: adjusting the pH value of the addition product to 4 or below 4, and separating to obtain an acidified product; step 3, cyclization reaction: carrying out cyclization reaction on the acidified product to obtain 1-propylene-1, 3-sultone; the catalyst is soluble metal salt which is soluble in water. According to the method, the catalyst and the free radical initiator which are low in price are compounded, so that a product with relatively good conversion rate and selectivity is obtained.

The application discloses a kind of diindole derivatives and preparation method thereof, it is left-handed or right-handed optical active body or racemate with the following structural formula;Its preparation includes with isoindoline group propargyl alcohol compound and 2-indole methanol compound as raw material, with organic phosphoric acid catalyst as catalyst, reaction is obtained in organic solvent diindole derivative.The application utilizes catalytic tandem reaction method to synthesize diindole derivative, reaction condition is mild, process is simple, operation is convenient, the potential fluorescent property and biological activity of obtained product, this will have important significance to fluorescent material and synthesis drug screening.

The invention relates to the field of organic synthesis, in particular to a preparation method of a 6-arylvinyl-6-phosphono-5, 6-dihydroindeno [2, 1-b] indole compound. The preparation method comprises the following steps: mixing an indole ring-containing benzene propargyl alcohol compound, a phosphine oxide compound, a catalyst and a solvent to obtain a mixture, and carrying out a cyclic isomerization reaction to obtain the 6-arylvinyl-6-phosphono-5, 6-dihydroindeno [2, 1-b] indole compound. The preparation method provided by the invention is wide in substrate application range, can be used for synthesizing compounds with different molecular structures, is mild in reaction condition, cheap and easily available in reagent, good in atom economy, simple and convenient in product post-treatment and high in yield, and is suitable for industrial production and promotion of practical application.

The present invention provides a catalyst for preparing dialkyl carbonates through the coupling reaction of a monohydric alcohol and CO2, a preparation method and application thereof, and a preparation method for symmetrical dialkyl carbonates, and relates to the technical field of organic synthesis. The catalyst of the present invention comprises an active component and a carrier; the active component is an oxide of an active metal; the active metal comprises cobalt, as well as gallium and / or indium; and the carrier comprises γ-Al2O3 or SiO2. The multiple components of the catalyst of the present invention interact with each other, which can effectively adjust the acidity and alkalinity of the catalyst. It is used for the "one-pot" reaction of a monohydric alcohol, carbon dioxide, and propargyl alcohol to prepare symmetrical dialkyl carbonates, and has high activity and high selectivity. The results of the examples show that the catalyst of the present invention has a conversion rate of 80 to 93% for monohydric alcohols and a selectivity for symmetrical dialkyl carbonates of 95 to 99%; the catalyst has good thermal stability and a long catalytic life, and its activity does not decrease significantly after continuous use for more than 360 hours.

The invention relates to a 2-aroyl-1, 5-diaryl-1, 5-pentanedione derivative and a synthesis method and application thereof.The synthesis method comprises the steps that 3-aryl propargyl alcohol and 1, 3-diaryl-1, 3-propanedione are subjected to a series Meyer-Schuster rearrangement / nucleophilic addition reaction in the presence of a first catalyst and a first organic solvent, and the 2-aroyl-1, 5-diaryl-1, 5-pentanedione derivative is obtained; the invention discloses a 1, 5-pentanedione derivative. Compared with the prior art, the 2-aroyl-1, 5-diaryl-1, 5-pentanedione derivative prepared by the preparation method disclosed by the invention has no substituent group at the position 3, has good fluorescence emission performance and metal ion recognition performance, can be used as an organic small molecule fluorescent material molecule, and is applied to the fields of metal ion detection, fluorescent probes and the like.