305 results about "Ethoxidine" patented technology

The present invention relates to a process for the preparation of (4S)-4-(4-cyano-2-methoxyphenyl)-5-ethoxy-2,8-dimethyl-1,4-dihydro-1,6-naphthyridine-3-carboxamide of formula (I) and to the preparation and use of crystalline modification I of (4S)-4-(4-cyano-2-methoxyphenyl)-5-ethoxy-2,8-dimethyl-1,4-dihydro-1,6-naphthyridine-3-carboxamide of formula (I).

The invention relates to the field of synergists, aims to solve the problems of crop phytotoxicity, environmental pollution and the like possibly caused by application of excessive herbicides, and provides a synergist which comprises the following components in parts by weight: 50-55 parts of ammonium sulfate, 27-37.5 parts of anhydrous sodium sulfate, 8-10 parts of a dispersing agent, 3-5 parts of potassium fulvate, 1-2 parts of a wetting agent and 0.5-1 part of ethyoxyl modified trisiloxane. The synergist obtained by compounding the raw materials can effectively improve the use effect of the herbicide; the dispersing agent can form a protective film on the surfaces of pesticide particles, so that the pesticide particles are prevented from being broken or agglomerated due to mutual collision, the surface tension between water and pesticide powder is reduced, and the solubility and stability of the pesticide are enhanced; ethyoxyl modified trisiloxane can promote pesticide components to be spread on the surfaces of plants quickly and uniformly, promote the pesticide components to permeate into the plants and accelerate the conduction effect of the plants, so that the effect of the pesticide is greatly improved; the growth promoter can promote the absorption of the plant to the pesticide and the conduction of the pesticide in the plant body.

The invention belongs to the technical field of flame-retardant master batches, and particularly relates to a flame-retardant master batch for polypropylene and a preparation method thereof.The preparation method comprises the steps that tris (2-hydroxyethyl) isocyanurate is heated and molten, tetrabutyl titanate and DOPO-DPP are added into the molten tris (2-hydroxyethyl) isocyanurate, the mixture reacts for 3-4 h, melamine and cyanuric acid are added into the molten tris (2-hydroxyethyl) isocyanurate, the mixture reacts for 30 min, cooling and smashing are conducted, and a macromolecular flame retardant TDMC is obtained; the preparation method comprises the following steps: carrying out ester exchange reaction on 2, 4-diphenyl-6-[2-hydroxy-4-(ethoxycarbonyl methoxy) phenyl]-1, 3, 5-triazine and 2, 2, 6, 6-tetramethyl piperidinol to prepare a free radical capturing agent; the polypropylene, the TDMC, the free radical scavenger and the zeolite are put into a high-speed mixer to be stirred and mixed, and then extrusion granulation is performed. The macromolecular flame retardant TDMC is adopted, the molecular weight of the macromolecular flame retardant TDMC is large, the water resistance is good, and the compatibility and damp-heat stability of the flame-retardant master batch in polypropylene are improved.

The invention discloses a molecular sieve catalyst for synthesizing methyl ethyl carbonate by a transesterification method and a regeneration method, and relates to the technical field of molecular sieve catalysts, the molecular sieve catalyst comprises a microporous double-active-center inner core and an amphoteric mesoporous shell; the microporous double-active-center core takes the X-type zeolite as a carrier to load potassium, cesium, lanthanum and barium; the amphoteric mesoporous shell is an MCM-41 and SBA-15 composite mesoporous silica layer coating the outer part of the inner core and has a double-mesoporous structure, amino propyl triethoxy silane and carboxyethyl triethoxy silane are grafted on the surface of the amphoteric mesoporous shell, and zirconium and titanium are co-doped. According to the invention, collaborative optimization of active centers and mass transfer channels is realized through a core-shell structure of a microporous double-active-center core and an amphoteric mesoporous shell. The activity and selectivity of catalytic transesterification are remarkably improved by the microporous core; due to the double-mesoporous structure and surface functional modification of the amphoteric mesoporous shell, the mass transfer efficiency of reactants and products is improved, and the adaptability of the catalyst to a reaction system is enhanced.

The application relates to the technical field of chemical synthesis, in particular to a synthesis method of a key intermediate of pentconazole, which comprises the following steps: S1, Witting-Horner reaction of 2,4-dichlorobenzophenone and (diethoxy) phosphoethyl acetate under the action of a strong base to generate 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester; S2, Prilezhaev epoxidation reaction of 3-(2,4-dichlorophenyl)-2-en-hexanoic acid ethyl ester and meta-chloro peroxybenzoic acid to generate 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester; and S3, base hydrolysis and acidification of 3-(2,4-dichlorophenyl)-2,3-epoxy-hexanoic acid ethyl ester to obtain a key intermediate 2-(2,4-dichlorophenyl) pentanal of pentconazole. The application has the effects of higher reaction yield, lower toxicity of reaction raw materials and more gentle reaction conditions.

Disclosed in the present invention is a monodisperse nanocalcium carbonate-based foliar calcium fertilizer, comprising the following raw materials in parts by mass: 1-20 parts of a monodisperse nanocalcium carbonate filter cake, 0.05-0.9 parts of ethoxy-modified polytrisiloxane, 0.01-0.8 parts of modified casein, 0.01-0.8 parts of an enzyme, 0.05-0.9 parts of a sugar alcohol, and 10-180 parts of water. After being diluted by means of water such that the solid content of calcium carbonate is 0.5-2%, the foliar calcium fertilizer is used for foliar calcium supplementation of various crops and fruit and vegetable crops. The novel foliar calcium fertilizer is safe and non-toxic, can be directly sprayed onto foliar and fruit surfaces of crops and fruits and vegetables, effectively ensures calcium absorption and utilization in crops, achieves the effect of increasing yield and increasing income, and can also improve the yield of fruits and vegetables.

The application discloses a preparation method of a key intermediate of dapagliflozin, and belongs to the technical field of preparation of medical intermediates. The preparation method of the key intermediate of dapagliflozin comprises the following steps: 1, 1-ethoxy-4-methylbenzene is prepared by using p-cresol, sodium hydroxide and diethyl sulfate; 2, (4-ethoxybenzyl) phenyl sulfide is prepared by using 1-ethoxy-4-methylbenzene, thiophenol, a palladium catalyst, an alkali and an oxidant; 3, 1-benzyl-4-ethoxybenzene is prepared by using (4-ethoxybenzyl) phenyl sulfide under a hydrogen atmosphere; 4, 4-ethoxy-2'-chlorobenzhydrol is prepared by carrying out chlorination reaction on 1-benzyl-4-ethoxybenzene; and 5, 5-bromo-2-chloro-4'-ethoxybenzhydrol is prepared by carrying out bromination reaction on 4-ethoxy-2'-chlorobenzhydrol. The yield and purity of 5-bromo-2-chloro-4'-ethoxybenzhydrol prepared by the method are higher, the process is safer, and the production cost is reduced.

The invention discloses a synthesis method of 4-bromo-3-(ethoxymethyl) benzoic acid, which comprises the following steps: (1) activating carboxyl of p-bromobenzoic acid serving as a raw material in the presence of an organic anhydride activator, and then performing chloromethylation reaction with paraformaldehyde in the presence of a chlorine-containing Lewis acid catalyst to obtain 4-bromo-3-(ethoxymethyl) benzoic acid; after the reaction is completed, carrying out post-treatment to obtain an intermediate 4-bromo-3-(chloromethyl) benzoic acid; and (2) carrying out nucleophilic substitution reaction on the intermediate obtained in the step (1) in ethanol under the action of inorganic alkali to prepare the target product 4-bromo-3-(ethoxymethyl) benzoic acid. According to the invention, through one-pot activation and chloromethylation of p-bromobenzoic acid, concise, efficient and highly economical synthesis from cheap raw materials to the sparsentan key intermediate is realized.

This invention discloses a yam oxylipoic acid compound with aromatase inhibitory activity, its application, and analytical identification methods, belonging to the field of medicinal chemistry. The yam oxylipoic acid compound is (Z)-9-ethoxy-6,10-dihydroxyoctadec-7-enoic acid, a novel compound. This compound can significantly inhibit aromatase activity and possesses the ability to inhibit excessive estrogen production, thus showing promising application prospects and value in diseases related to estrogen imbalance regulation.

Disclosed is a method for preparing oxetan-2-ylmethanamine, which belongs to the field of organic synthesis. [2-(1-ethoxyethoxy)methyl]propylene oxide is used as an initial raw material, and reacted in the presence of potassium tert-butoxide and trimethylsulfoxonium iodide; the resulting product is reacted with a sulfonyl compound and triethylamine; the resulting product is reacted with a compound of phthalimide; the resulting product is reacted with an amino group-containing compound, to obtain oxetan-2-ylmethanamine. The method according to the disclosure allows for an overall yield of not less than 30% in scale-up production (kilogram level), which is higher. Moreover, compared with the traditional method for preparing oxetan-2-ylmethanamine, a palladium-carbon catalytic hydrogenation step is not required, and dangerous chemical-sodium azide is not required in the method according to the disclosure. Thus, the method has high safety, low production cost, simple operations, and thereby is suitable for industrial production.

The invention relates to the technical field of chemical synthesis, and particularly discloses a compound with a peculiar smell removing function as well as a preparation method and application thereof. The chemical name of the compound is 2-ethoxy-3-((E)-methoxy-3-oxopropyl-1-alkene-1-yl) phenyl cinnamate, the smell of the compound is extremely light, sulfur-containing and nitrogen-containing compounds causing stink can be captured through a Michael addition reaction, and efficient peculiar smell removal is achieved. The preparation method comprises the following steps: (1) taking cinnamic acid as an initial raw material, and reacting with diethylamino sulfur trifluoride to prepare cinnamic acid acyl fluoride; (2) carrying out an esterification reaction on the cinnamic acid acyl fluoride and 2-methoxy-3-hydroxybenzaldehyde in the presence of 4-dimethylaminopyridine, so as to obtain 2-methoxy-3-formyl phenyl cinnamate; and (3) carrying out Wittig reaction on the 2-methoxy-3-formyl phenyl cinnamate and a phosphorus ylide reagent, so as to obtain the target compound.

The invention discloses a preparation method of a dapagliflozin intermediate 5-bromine-2-chlorine-4 '-ethyoxyl diphenylmethane, which comprises the following steps: carrying out nucleophilic substitution reaction on 4-bromine-1-chlorine-2-fluorobenzene and 4-ethyoxyl phenylacetate, and then hydrolyzing and decarboxylating to obtain the dapagliflozin intermediate 5-bromine-2-chlorine-4'-ethyoxyl diphenylmethane. By optimizing the preparation route, the reaction utilization rate, the product yield and the product purity of the raw materials are improved, high-risk and high-pollution chemicals are prevented from being used, and the method is convenient to operate, safe, environmentally friendly, efficient in reaction and beneficial to industrial implementation.

The invention relates to the technical field of pesticide production, and particularly discloses a preparation process of glufosinate-ammonium intermediate 3-(methyl hydroxyl phosphonyl) propionaldehyde. The preparation method comprises the following steps: 1, carrying out addition reaction on diethyl methylphosphonite and acrylic acid in absolute ethyl alcohol to generate 3-[ethyoxyl (methyl) phosphonyl] propionate; in the second step, 3-[ethyoxyl (methyl) phosphonyl] propionate is subjected to a hydrosilylation reaction in an oriented mode, and 3-triethyl siloxy-3-ethyoxyl propyl methyl ethyl phosphonate is generated; and 3, carrying out a simple dilute acid hydrolysis reaction to obtain the 3-(methyl hydroxyl phosphonyl) propionaldehyde. According to the method, a three-step reaction route of addition-hydrosilylation-hydrolysis is adopted, and the acrylic acid is used for replacing the traditional high-toxicity raw material acrolein, so that the toxicity risk is avoided from the source, the yield of the target glufosinate-ammonium intermediate is remarkably improved, the total yield of the three-step reaction can reach 95% or above, and the method is suitable for industrial production. And an efficient and green brand-new technical scheme is provided for large-scale production of glufosinate-ammonium.

This invention relates to a method for preparing the fenelone intermediate 2-cyanoethyl(4S)-4-(4-cyano-2-methoxyphenyl)-5-ethoxy-2,8-dimethyl-1,4-dihydro-1,6-naphthidine-3-carboxylic acid ester, and also relates to diastereomeric salts (Va), (Vb), (Vc), and / or (Vd). This method is simple to operate, and the diastereomeric salts can be obtained with very high chemical and enantiomeric purity (tartrate ester content <0.05%) through a single dissociation, avoiding the raw material loss and waste problems caused by multiple dissociations. It also has low production costs and meets the requirements of green production.

The invention discloses a hydrophobic Zr-doped SiO2 (at) APTES-T composite aerogel desulfurization adsorbent as well as a preparation method and application of the hydrophobic Zr-doped SiO2 (at) APTES-T composite aerogel desulfurization adsorbent. The preparation method comprises the following specific steps: dissolving thiophene in n-heptane to form a non-polar template solution, and adding the non-polar template solution into a polar mixed solution of ZrOCl2, methyltriethoxysilane and 3-aminopropyltriethoxysilane, wherein water and ethanol serve as solvents of the ZrOCl2, the methyltriethoxysilane and the 3-aminopropyltriethoxysilane; the non-polar template solution is stirred in the polar solution to form uniform tiny liquid drops. The preparation method comprises the following steps: carrying out a hydrolysis-polymerization reaction on a mixed solution to form hydrophobic Zr-doped SiO2 (at) APTES-T alcogel, carrying out aging, replacement and drying steps to obtain the hydrophobic Zr-doped SiO2 (at) APTES-T composite aerogel desulfurization adsorbent, and applying the hydrophobic Zr-doped SiO2 (at) APTES-T composite aerogel desulfurization adsorbent to adsorption removal of thiophene compounds in simulated aromatic hydrocarbons. Results show that the desulfurization adsorbent disclosed by the invention has good adsorption performance on thiophene sulfides in aromatic hydrocarbons, has excellent performance of resisting competitive adsorption of polar impurities, and has good application prospects in the field of deep desulfurization.

The invention belongs to the technical field of medicine synthesis, and particularly relates to a method for efficiently preparing cyclobutane derivatives. Comprising the following steps: dissolving 4-chloro-7H-pyrrolo [2, 3-d] pyrimidine and chloromethyl pivalate in 1, 4-dioxane, and adding an acid binding agent for reaction to obtain a reaction solution; the preparation method comprises the following steps: adding 1-(1-ethoxyethyl)-4-pyrazol boronic acid pinacol ester, purified water, a catalyst and an acid-binding agent into a reaction kettle, carrying out Suzuki reaction, separating liquid, adding activated carbon into an upper organic phase for decoloration, adding an organic solution containing hydrogen chloride for crystallization, and filtering to obtain a wet product; and dissolving the wet product and 2-[1-(ethylsulfonyl)-3-azacyclobutane] acetonitrile in 1, 4-dioxane, and reacting under an alkaline condition to obtain the cyclobutane derivative. According to the preparation method, synthesis is performed through a one-pot four-step reaction, a solvent only relates to 1, 4-dioxane and water, and post-treatment is simple, convenient and efficient.

The present invention relates to an isoindoline compound containing a phenylethoxyalkyleneamine structure, a conjugate thereof, and use thereof. The isoindoline compound containing a phenylethoxyalkyleneamine structure has a structure represented by formula (I). The conjugate thereof has a structure represented by formula (B). The compound of the present invention exhibits increased proliferation inhibition activity for cancer cells and a degradation effect on proteins such as GSPT1, demonstrating practical values.

The invention provides a novel economical and practical method for preparing the quetiapine key intermediate 1-[2-((2-hydroxy ethyoxyl) ethyoxyl) ethyl] piperazine hydrochloride.

The invention belongs to the field of biological medicines, and discloses an (R)-3-(1-([1, 1 '-biphenyl]-2-yl) ethyoxyl) pyridine-2-amine derivative as well as a synthesis method and application thereof. A compound with a structure as shown in a general formula I of the derivative or pharmaceutically acceptable salt, hydrate, solvate, polymorphic substance, tautomer, stereoisomer, isotope derivative or prodrug thereof has higher ROS1 or ALK protein kinase inhibitory activity; the compound has high anti-proliferative activity on human non-small cell lung cancer and solid tumors such as brain metastatic tumors, glioblastoma and breast cancer, and can be used for preparing drugs for treatment and / or prevention and / or delay and / or adjuvant treatment and / or treatment of tyrosine protein kinase, especially diseases mediated by ROS1 and ALK kinase and mutant kinase thereof.

The invention discloses a method for directly preparing a racemic oxidation product from a fennerenone enantiomer through photocatalysis, and belongs to the technical field of organic synthesis.The method comprises the steps that an R-type fennerenone isomer is taken to be placed in a reaction bottle, a photosensitizer containing iridium or ruthenium is added, and a solvent is added at the speed of 0.1 M in the air atmosphere; the method comprises the following steps: dissolving 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-2, 8-dimethyl-1, 6-naphthyridine-3-formamide in a solvent, stirring, transferring a mixture into a photoreactor of a blue light LED (Light Emitting Diode) with the wavelength of 455-465 nm, stirring, transferring a mixed solution after the reaction is finished into a round-bottom flask, purifying a volatile solvent to obtain a product 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-2, 8-dimethyl-1, 6-naphthyridine-3-formamide, and carrying out chiral HPLC (High Performance Liquid Chromatography) analysis on the product. High temperature, high pressure or a strong oxidant is not needed, and reaction conditions are mild; oxygen in air is oxidized at room temperature, so that energy consumption and pollutant generation are reduced; compared with the traditional oxidation condition, the method does not need to undergo the process of oxidation first and then high-temperature induced racemization, and the racemization product can be directly obtained.

The application discloses a method for preparing N-ethoxyl oxalyl alanine ester by using a dynamic tubular reactor, which comprises the following steps: (1) reacting L-alanine, diethyl oxalate and 4-dimethylaminopyridine in the dynamic tubular reactor; (2) removing light components from the reaction solution; (3) reacting the reaction solution after removing the light components and ethanol in the dynamic tubular reactor; and (4) obtaining N-ethoxyl oxalyl alanine ester after removing the light components. Compared with traditional kettle reactors and tubular reactors, the method adopts the dynamic tubular reactor to prepare N-ethoxyl oxalyl alanine ester, and through the regulation of reaction parameters, the selectivity of key by-products N-oxamide and double N-oxamide can be effectively controlled below 2%. The process has the advantages of high reaction yield, high degree of continuous operation, significantly shortened reaction time and no use of high-toxicity materials such as benzene.

This invention discloses a green synthesis process for 2-chloropyranose-1-yl)-4'-ethoxydiphenylmethane, belonging to the field of pharmaceutical intermediate preparation. The method involves forming a mixture of a substrate in the protected state of Formula I and a reducing agent containing siloxane bonds, which is continuously fed into a microreactor loaded with a confined-domain MOF (Metal-Oxide-Fractions) supported catalyst for room-temperature reduction. The MOF catalyst has a rigid pore size of 1.2~2.5 nm and internally coordinates and anchors metal trifluoromethanesulfonate. This invention utilizes the limiting confinement effect of rigid channels to lock the substrate conformation, blocking the surface attack of reactants and achieving extremely high configuration selectivity. Simultaneously, the efficient mass transfer of the continuous flow microchannel and the online infrared spectroscopy closed-loop control system completely eliminate the need for traditional cryogenic conditions, remove highly corrosive fluorine-containing waste liquid, significantly reduce synthesis costs, and achieve efficient, green, and stable continuous industrial production of this core intermediate.

The invention discloses a glyphosate soluble concentrate and a preparation method, and the glyphosate soluble concentrate comprises the following raw material components in parts by weight: 30-40 parts of glyphosate, 10-15 parts of isopropylamine, 8-12 parts of a composite synergist, 2-3 parts of an anti-freezing agent, 0.05-0.1 part of a pH regulator, 2-3 parts of an additive, 0.1-0.5 part of a defoaming agent, 1-2 parts of a loading agent and 40-50 parts of water. Compared with the prior art, the glyphosate soluble concentrate prepared by the invention has the advantages that the propoxylated quaternary ammonium salt and the ethyoxyl alkyl phosphate are mixed according to a certain mass ratio to form the synergist, so that the pesticide effect of glyphosate is remarkably improved. Meanwhile, the aluminum pillared clay is introduced to load the glyphosate and is cooperatively used with the polydopamine-sodium alginate compound, so that the prepared glyphosate soluble concentrate has relatively high leaf deposition rate and rain wash resistance and also has excellent ultraviolet resistance.

The invention relates to a synthesis method of 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-1, 4-dihydro-2, 8-dimethyl-1, 6-naphthyridine-3-formamide, which comprises the following four steps: carrying out a Knoevenagel condensation reaction, carrying out a Hantzsch dihydropyridine synthesis method, carrying out an O-ethylation reaction and carrying out a deprotection reaction to synthesize the 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-1, 4-dihydro-2, 8-dimethyl-1, 6-naphthyridine-3-formamide, and carrying out a reaction to obtain the 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-1, 4-dihydro-2, 8-dimethyl-1, 6-naphthyridine-3-formamide. The preparation method of the 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-1, 4-dihydro-2, 8-dimethyl-1, 6-naphthyridine-3-formamide has the advantages that the selectivity is high, the post-treatment is simple, the yield and the purity of the product are high, a new synthesis route and method are developed for synthesizing the 4-(4-cyano-2-methoxyphenyl)-5-ethoxy-1, 4-dihydro-2, 8-dimethyl-1, 6-naphthyridine-3-formamide, the amplified production is conveniently realized, and the method is suitable for industrial production. The method has good application potential and research value.

The invention discloses a synthesis method of m-acetoxystyrene, which is characterized by comprising the following steps: adding m-hydroxybenzaldehyde, vinyl ethyl ether and trifluoroacetic acid into an organic solvent A, and reacting in an inert gas atmosphere to obtain a reaction solution; dropwise adding the reaction solution into a Wittig reagent, carrying out a reaction, and carrying out post-treatment, so as to obtain 1-(1-ethyoxyl ethyoxyl)-3-vinyl benzene; the Wittig reagent is prepared by dispersing methyl triphenyl phosphorus bromide and sodium methoxide in an organic solvent B; the preparation method comprises the following steps: adding 1-(1-ethoxyethoxy)-3-vinylbenzene, an acid solution and an acetylation reagent into a solvent to react, and preparing m-acetoxystyrene after the reaction. The method is simple in process step, mild and controllable in reaction condition, high in equipment universality, low in comprehensive production cost, capable of effectively inhibiting side reactions and improving the product quality, suitable for industrial production and high in practicability.

This invention discloses a yam component with α-glucosidase inhibitory activity, its application, and analytical identification methods, belonging to the field of medicinal chemistry. The yam component is (Z)-6-ethoxy-9,10-dihydroxyoctadecano-7-enoic acid, a novel compound extracted from yam, exhibiting excellent α-glucosidase inhibitory activity, thus showing promising application prospects and value in lowering blood sugar.

The present application relates to a preparation method of cyprosulfamide, and the cyprosulfamide is prepared by using a one-pot method, and the method specifically comprises the following steps: adding an organic base, a reaction solvent, 2-chloro-3-(2,2,2-trifluoroethoxy)methyl-4-methylsulfonylbenzoic acid and a Curtius condensing agent into a reaction container, heating and refluxing for 3-5 h to generate an active ester intermediate; after the reaction solution containing the active ester intermediate is cooled, 1,3-cyclohexanedione and acetone cyanohydrin are added to perform a condensation rearrangement reaction, and cyprosulfamide is generated. The one-pot synthesis process is adopted, the use of dimethyl sulfoxide is avoided, compared with a traditional process, the method is green, environmentally friendly, has low safety risks, has high yield and good purity, and is more suitable for industrialized production.

The presently claimed invention relates to an alkaline composition for cleaning a substrate comprising i) copper or copper alloy and ii) cobalt or cobalt alloy, the composition comprising: a) at least one pH adjustor selected from diglycolamine, 4,4-diethoxy-N,N-dimethyl-1-butanamine, 3-dimethylaminopropan-1-ol, dimethylaminoethoxyethanol, N,N-dimethylisopropanolamine, ethylethanolamine, N-methyldiethanolamine, 2-(2-(methylamino)ethoxy)ethanol, 3-(methylamino)propane-1,2-diol, 2-[2-[2-(2-methoxy- ethoxy)ethoxy]ethoxy]ethylamine, 2-[2-(2-aminoethoxy)-ethoxy]-ethanol, N-butyldiethanolamine, diisopropanolamine, N-methyldiisopropanolamine, monoethanolamine, 3-dimethylamino-1,2-propandiol, 2- amino-1-butanol, 2-(2-(2-(2-aminoethoxy)ethoxy)ethoxy)ethanol, prolinol, 1-methyl-2-pyrrolidinemethanol, 1-methyl-2-pyrrolidinemethanol, 1-methyl-3-pyrrolidinol, 2-amino-2-methyl-1-propanol, N,N-dimethylethanolamine, butylethanolamine, diethylethanolamine, 3-methoxypropylamine, 4-(2-hydroxyethyl)morpholine, 4-(dimethylamino)cyclohexanol, 2-amino-2-methyl-1, 3-propanediol, or diisopropylamine; b) at least one complexing agent selected from C2 to C12 hydrocarbon having at least two sulfonic acid or carboxylic acid groups; c) at least one polymeric dispersing agent having a weight average molecular weight ≥ 1000 g / mol; and d) a solvent comprising water.

The present application provides methods for preparing (R)-4-(3-((S)-1-(4-amino-3-methyl-1H-pyrazolo[3,4-d]pyrimidin-1-yl)ethyl)-5-chloro-2-ethoxy-6-fluorophenyl)pyrrolidin-2-one, which is useful as a phosphoinositide 3-kinase-delta (PI3Ks) inhibitor, as well as salt forms and intermediates related thereto.

The present invention discloses an A,A'-bipyridinehydrazone-functionalized conjugated pillar[5]arene macrocyclic molecule and a synthesis method thereof. The invention comprises reacting a bis(4-formylphenylboronic acid)-functionalized pillar[5]arene with 2-hydrazinepyridine through an imine condensation reaction to obtain an A,A'-bipyridinehydrazone-functionalized conjugated pillar[5]arene PYP5 having two rigid functional arms. The macrocyclic molecule PYP5 can self-assemble through multiple hydrogen bonds to form a supramolecular polymer network. Thanks to the "double-arm-macrocyclic synergistic effect" between the double arms of the pillar[5]arene and the ethoxy group, PYP5 can provide multiple "clustered hydrogen bonds" to tightly bind ClO4. − Therefore, the supramolecular polymer network can effectively treat ClO4 in water. − It can show good adsorption and separation performance and can effectively remove ClO4 in water − The removal rate can reach 99.24%. The A,A'-bispyridinehydrazone functionalized conjugated column[5] aromatic macrocyclic molecule provided by the present invention has good application prospects in the fields of supramolecular assembly, water pollutant removal, adsorption separation, etc.