38 results about "Oxepane" patented technology

This invention relates to the compound (2R)-2-(6-{5-chloro-2-[(oxan-4-yl)amino]pyrimidin-4 -yl}-1-oxo-2,3-dihydro-1H-isoindol-2-yl)-N-[(1S)-1-(3-fluoro-5-methoxyphenyl)-2-hydroxyethyl]propanamide, and in particular to novel physical forms of the compound, a process for preparing the compound and synthetic intermediates for use in the process, and novel formulations containing the compound, as well as therapeutic uses of the compound.

A polystyrene-based chalcone including units of a 1-(2H-1,3-benzodioxol-5-yl)-3-[4-(dimethylamino)phenyl]-(2E)-propane-1-one and units of a 2-hydroxyethyl methacrylate. The units of the 1-(2H-1,3-benzodioxol-5-yl)-3-[4-(dimethylamino)phenyl]-(2E)-propane-1-one and the units of the 2-hydroxyethyl methacrylate are in a matrix of a polystyrene. A process for preparing the polystyrene-based chalcone and application as a laser medium with fine coating characteristics.

The invention belongs to the technical field of medical chemistry, and relates to a preparation method of ticarcillin sodium side chain 3-ATMA. The method comprises the following steps: adding thiophenemalonic acid and acetone into a reactor at 20-60 DEG C, and dissolving; then, cooling to 0-10 DEG C, adding zinc chloride and anhydride, heating to 15-40 DEG C, and carrying out heat preservation reaction for 10-20 hours; the preparation method comprises the following steps: adding 2, 2-dimethyl-5-(3-thienyl)-1, 3-dioxane-4, 6-diketone into a reaction kettle, adding purified water for hydrolysis after the reaction is completed, continuously stirring for reaction, and then filtering, washing and drying to obtain the ticarcillin sodium side chain 2, 2-dimethyl-5-(3-thienyl)-1, 3-dioxane-4, 6-diketone. The preparation method disclosed by the invention is simple and convenient to operate, the used materials are safer, the technological process is green and environment-friendly, and the 3-ATMA is high in yield and good in quality.

The invention relates to a process for the preparation of 1-(1,3-benzodioxol-5-yl)-1-propanone comprising the step of reacting 3,4-dimethylendioxybenzene with propionic anhydride in the presence of a bulk or supported catalyst, being said catalyst selected from the group of a sulphonated cross-linked divinylbenzene resin, a sulphonated cross-linked divinylbenzene resin partially exchanged with iron, zinc or gallium, a perfluorinated sulphonic resin, and a perfluorinated sulphonic resin partially exchanged with iron, zinc or gallium, wherein said catalyst has an average particle size from 1 μm to 300 μm, preferably from 1 μm to 180 μm, more preferably from 1 μm to 100 μm as measured with DLS (Dynamic light scattering) or a granulometer. The process is advantageously carried out at stoichiometric ratio between the reagents and with a continuous process.

The present invention relates to a process for the preparation of trioxane derivatives.

The invention belongs to the technical field of synthesis of organic compounds, and relates to a synthesis method of ticarcillin sodium. The synthesis method comprises the following steps: a condensation reaction step: in a nitrogen atmosphere, in an organic solvent and in the presence of N, N-bis (trimethylsilyl) urea, carrying out a reaction on 6-aminopenicillanic acid and 2, 2-dimethyl-5-(3-thienyl)-1, 3-dioxane-4, 6-diketone to generate ticarcillin, and filtering to obtain a solution containing ticarcillin; and a salt forming reaction step: carrying out a one-step salt forming reaction on the obtained solution containing ticarcillin and a sodium isooctanoate solution to obtain ticarcillin sodium. In the synthesis process, no acid or alkali is used for adjusting the pH value, so that open-loop degradation of a lactam ring in a ticarcillin structure is avoided; no water is added in the synthesis process, an organic solvent is used in the whole process, and other impurities generated by hydrolysis reaction are avoided; meanwhile, tedious steps such as extraction or reduced pressure distillation are not needed, the preparation process is easy and convenient to operate, the yield is high, the purity is high, and large-scale production is easy.

This invention relates to a process for preparing compounds having formula (I): R 1 ‑C(=O)‑O‑CH2‑O‑C(=O)‑R 2 (I), where R 1 and R 2 Each of the terms represents an alkyl, cycloalkyl, or aryl group independently, wherein the alkyl, cycloalkyl, or aryl group is optionally substituted; the process includes step i) reacting the following substances: compound A selected from: trioxane, polyoxymethylene without a hydroxyl terminal group; compound (II): R 1 -C(=O)-O-C(=O)-R 2 (II); and perfluorosulfonic acid; wherein step i) is carried out at a temperature T1 of at least 50°C, wherein the molar ratio of compound (II) to compound A is 1:1 to 1.2:1.

The present invention relates: to a tablet formulation comprising crystalline Hydrate 1 Modification A form of the compound 3-(3-chloro-2-methoxy-anilino)-2-[3-[[(2S)-l,4-dioxan-2-yl]methoxy]-4-pyridyl]-1, 5,6,7- tetrahydropyrrolo[3,2-c]pyridine-4-one, of formula (A): wherein the content of water is greater than 0% (w / w), particularly greater than 0% and less than or equal to 4%, of the total weight of said compound of formula (A); to methods of preparing said tablet formulation, and to uses of said tablet formulation in the prophylaxis and / or treatment of diseases.

The present invention relates to a method for producing a compound represented by the following formula (I), which comprises a step of subjecting a compound represented by the following formula (II) and a compound represented by the following formula (III) to an aldol condensation reaction in the presence of [1] a compound represented by the following formula (I) and [2] a compound represented by the following formula (IV): TIFF0007773005000076.tif1968 The present invention relates to [3] a method for producing a compound represented by the following formula (VI), which comprises a step of subjecting a compound represented by the following formula (V) to a reduction reaction together with an ammonia equivalent. TIFF0007773005000077.tif2144

A process for preparing trioxane from methanol includes: step 1: subjecting a mixture of methanol and methylal to a reaction to obtain formaldehyde, and absorbing the formaldehyde with water to obtain a concentrated formaldehyde aqueous solution; step 2: subjecting the concentrated formaldehyde aqueous solution to cyclization to obtain a mixture containing trioxane, and passing the mixture through a trioxane concentration tower to obtain a crude trioxane product; step 3: converting a by-product and unreacted formaldehyde in the crude trioxane product into methanol, conducting dehydration through a membrane dehydration process, and subjecting a retentate to dealcoholization to obtain purified trioxane; and step 4: subjecting the remaining streams to reactive distillation to obtain a mixture of methanol and methylal at a top- and water at a bottom of the reactive distillation tower; returning the mixture of methanol and methylal to step 1; and returning or discharging the water.

The method for producing a polyacetal copolymer according to the present invention is a method for producing a polyacetal copolymer by copolymerizing trioxane and a comonomer capable of copolymerizing with the trioxane in the presence of a polymerization catalyst. The polymerization catalyst is a heteropolyacid (A) and a heteropolyacid salt (B), and the heteropolyacid (A) and the heteropolyacid salt (B) are used in a mixed manner.

The present application relates to carbon dioxide absorbent technical field, especially relates to a kind of ionic liquid-like carbon dioxide absorbent preparation method.The present application includes the following steps: (one) synthesis preparation: the choline chloride and urea are made into low eutectic solvent DES, polyamide amine PAMAM G1 and low eutectic solvent DES are made into absorbent;(two) mixing and heating: after drying raw material is added to heating container, add dioxane as solvent, place in oil bath, stirring heating, mixture gradually from turbid solid becomes homogeneous, transparent, viscous liquid;(three) purification and water removal: after forming homogeneous liquid, in vacuum stirring, to remove moisture, and the final product is liquid ionic liquid carbon dioxide absorbent.The beneficial effect is: the preparation method of the present application is simple and controllable, reaction condition is mild, easy to scale production, provides a feasible technical scheme for industrial application;Solve the existing absorbent active site few, the problem of low carbon dioxide capture amount.

Provided is a pharmaceutical composition containing 6-ethyl-3-{3-methoxy-4-[4-(4-methylpiperazin-1-yl)piperidin-1-yl]anilino}-5-[(oxan-4-yl)amino]pyrazine-2-carboxamide or a pharmaceutically acceptable salt thereof and a sweetener for reducing the bitterness of gilteritinib, suppressing the decrease in dissolution stability of gilteritinib due to, for example, stress such as heat and / or humidity over time, and having excellent dissolution stability. The pharmaceutical composition contains gilteritinib or a pharmaceutically acceptable salt thereof, a sweetener, and sugars and / or sugar alcohols.

The invention relates to a crystal form A of(S)-2-(3S,8S)-3-(4-(3,4-dichlorobenzyloxy)phenyl-7-((S)-1-phenylpropyl)-2,3,6,7,8,9-hexahydro-[1,4]-dioxino[2,3-g]isoquinolin-8-ylformylamino)-3-(4-(2,3-dimethylpyridin-4-yl)phenyl)propionic acid (“OAD2”), and methods of preparation thereof. Crystal form A may be useful in the treatment of various conditions and metabolic disorders including, but not limited to, type 2 diabetes.

To provide an efficient method for producing (2R)-1-(morpholin-4-yl)-2-[(oxan-2-yl)oxy]propan-1-one.SOLUTION: In one aspect, there is provided a method for producing (2R)-1-(morpholin-4-yl)-2-[(oxan-2-yl)oxy]propan-1-one. This production method comprises contacting (2R)-2-hydroxy-1-(morpholin-4-yl)propan-1-one and 3,4-dihydro-2H-pyran in the presence of pyridinium paratoluenesulfonate at a temperature of 40°C or higher.SELECTED DRAWING: None

The invention relates to the technical field of synthetic methods of methyl acetate, in particular to an ECR-1 zeolite catalyst as well as a preparation method and application thereof. The preparation method of the ECR-1 zeolite catalyst comprises the following steps: A) stirring and mixing an aqueous solution containing a sodium source and an aluminum source, trioxane and colloidal silicon dioxide to obtain a mixed solution; (B) carrying out rotary crystallization on the mixed solution and the mixture at 120-150 DEG C; the mixture is prepared from SiO2, Al2O3, TOX, Na2O and H2O; c) filtering and drying the mixture subjected to rotary crystallization, and calcining to obtain Na-ECR-1; and D) carrying out ion exchange on the Na-ECR-1 and an ammonium nitrate solution at 70-90 DEG C, washing, drying and calcining to obtain the ECR-1 zeolite catalyst. The prepared ECR-1 zeolite catalyst can be used as a catalyst for catalyzing carbonylation of dimethyl ether to synthesize methyl acetate, and has excellent catalytic performance.

The object of the present invention is to provide: a method for manufacturing a polyacetal copolymer having a good appearance of a molded product formed by a polyacetal copolymer and small differences between each product. The object of the present invention is achieved by the following. A method for manufacturing a polyacetal copolymer, which has at least the following steps in sequence: step (A), using trioxane as the main monomer (a), using at least one selected from a cyclic formal having at least one carbon-carbon bond and a cyclic ether as a comonomer (b), adding a protonic acid polymerization initiator (c) and a molecular weight regulator (d1) according to the situation, and polymerizing a polyacetal copolymer in a polymerization machine; step (B), taking the polyacetal copolymer obtained in the aforementioned step (A) out of the polymerization machine, adding the aforementioned liquid molecular weight regulator (d2) having a boiling point lower than 200°C, and adjusting the molecular weight of the aforementioned polyacetal copolymer; and, step (C), immediately following the step of adjusting the molecular weight, deactivating the aforementioned polymerization initiator (c).

The present invention relates: to the crystalline Hydrate 1 Modification A form of the compound 3-(3-chloro-2-methoxy- anilino)-2-[3-[[(2S)-1,4-dioxan-2-yl]methoxy]-4-pyridyl]-1,5,6,7-tetrahydropyrrolo[3,2- c]pyridine-4-one of formula (A): 5 *x H 2 O (A), wherein the content of water is greater than 0 % (w / w) and ≤ 4.0 % (w / w); • to a method of preparing said crystalline Hydrate 1 Modification A form of said compound of formula (A) and to intermediate compounds used in said method;• to pharmaceutical compositions and combinations comprising said crystalline Hydrate 1 Modification A form of said compound of formula (A); and • to said crystalline Hydrate 1 Modification A form of the compound of formula (A), and to pharmaceutical compositions or combinations comprising same for use in the treatment or prevention of a cancer, such as lung cancer, particularly non-small cell lung carcinoma.

Provided are a pharmaceutically acceptable salt and a crystalline form of a GLP-1 receptor agonist and a preparation method therefor. Specifically, provided are a pharmaceutically acceptable salt and a crystalline form of a compound 2-((4-((S)-3-(4-chloro-2-fluorophenyl)-2,3-dihydrobenzo[b][1,4] dioxane-5-yl)piperidin-1-yl)methyl)-1-(((S)-oxe-tane-2-yl)methyl)-1H-benzo[d]imidazole-6-formic acid.

The present application discloses a method for preparing a cigarette paper additive, comprising the following steps: 1) extracting ground wood lignin in a cigarette rod using a 1,4-dioxane-water solution; 2) mixing ground wood lignin with silk fibroin, treating with a composite enzyme, and obtaining a lignin-silk fibroin complex, which is an additive. The present application also provides a cigarette paper additive. The present application also provides a plugging paper using the above-mentioned cigarette paper additive and a method for preparing the same. The method provided in the present application is reasonable and easy to operate. The cigarette paper additive prepared in the present application can be added as a filler during the production of the plugging paper, and has the aroma of tobacco, antibacterial properties, and the like, and can greatly enhance the experience and antibacterial properties of cigarettes when smoking.

The present invention relates to a process of preparation of a compound having formula (I):wherein R1 and R2 represent, independently of each other, an alkyl, a cycloalkyl or an aryl group, said alkyl, cycloalkyl or aryl group being optionally substituted;said process comprising a step i) of reacting:a compound A selected from the group consisting of: trioxane, polyoxymethylene deprived of hydroxyl end groups;a compound of formula (II):anda perfluorosulfonic acid;wherein step i) is carried out at a temperature T1 of at least 50° C., wherein the molar ratio of compound of formula (II): compound A ranges from 1:1 to 1.2:1.

To provide a method for producing a polyacetal copolymer capable of obtaining a polyacetal copolymer having excellent hue and thermal stability, even when a polyacetal copolymer is produced using a protic acid as a polymerization catalyst.SOLUTION: There is provided a method for producing a polyacetal copolymer which comprises: a step of obtaining a crude polyacetal copolymer by copolymerization of trioxane as a main monomer (a) and a compound copolymerizable with trioxane as a comonomer (b), using a protic acid as a polymerization catalyst (c); a step of obtaining a mixture by mixing the crude polyacetal copolymer and a cyclic compound (d) containing an oxygen atom in the ring; and a step of feeding the mixture into an extruder to melt-knead while adding a predetermined basic compound (e) to the mixture.SELECTED DRAWING: None

The present disclosure relates to a method for preparing a benzodioxane or salts thereof. Specifically, the method of the present disclosure comprises a step of reacting a compound of formula E under the presence of a tri-substituted phosphine / azodicarboxylate to form a compound of formula F.

The invention relates to the technical field of lithium metal battery electrolytes, in particular to an electrolyte, application thereof and a cathode-free lithium metal battery. The invention provides an electrolyte. The electrolyte comprises a lithium salt, a solvent, a diluent and an additive, the diluent comprises a 1, 3-dioxane derivative, acetal carbon located at the position 2 in the 1, 3-dioxane of the 1, 3-dioxane derivative is substituted by Rf1 and Rf2, and the Rf1 and the Rf2 are the same or different; the Rf1 and the Rf2 are independently fluorine substituted alkyl groups; the additive is prepared from one or more of 1, 3, 5-trioxane, a derivative of the 1, 3, 5-trioxane and paraldehyde, and the additive is prepared from one or more of 1, 3, 5-trioxane, a derivative of the 1, 3, 5-trioxane and paraldehyde. The electrolyte can give consideration to both excellent ion transmission and lithium deposition dynamic performance under a low-temperature condition.

The invention relates to a synthesis method of 4H-benzo [d] [1, 3] dioxane-4-ketone and a derivative thereof, salicylic acid and the derivative thereof can easily realize various functional reactions, because the salicylic acid and the derivative thereof widely exist, have abundant reaction sites and are low in price, the synthesis method is undoubtedly a simple organic synthesis strategy. Salicylic acid and derivatives thereof not only can be subjected to simple coupling reaction with R-NH2 and R-X, but also can be subjected to reaction with CH2X2 to synthesize 4H-benzo [d] [1, 3] dioxane-4-ketone, and in the air atmosphere, the reaction temperature is reduced, and the reaction time is shortened. Bis (triphenylphosphine) nickel chloride (20mol%) is used as a catalyst, triphenylphosphine (0.5 equivalent) is used as a ligand, cesium carbonate (1.5 equivalent) is used as alkali, ethyl acrylate (4.0 equivalent) is used as an additive, and a target product is formed through reaction at 90 DEG C for 16 hours. According to the scheme reported by the invention, the conditions are simple, the raw materials are cheap and easy to obtain, the reaction can be directly carried out in the air atmosphere without external gas, the method has step and atom economy, and various 4H-benzo [d] [1, 3] dioxane-4-ketone and derivatives thereof can be effectively obtained.

The present invention relates to the use of 1,3-dioxolan-4-ones and 1,3-dioxan-4-ones of the formula (I)wherein R1 to R4 are as defined in the claims and the description, as aroma ingredients. Said compounds are used to impart an aroma impression, in particular a fragrance to a composition and also for enhancing and / or modifying the aroma, especially fragrance, of a composition. The present invention is further directed to a method of imparting an aroma to a composition by incorporating said compounds into the composition, to a composition comprising at least one of said compounds, and to specific 1,3-dioxolan-4-ones and 1,3-dioxan-4-ones.

The application discloses a benzo[b]oxepane compound and application thereof, and belongs to the technical field of medicines.The structural general formula of the compound is shown as formula (I).The compound has high androgen receptor antagonistic activity, and can effectively inhibit androgen-induced downstream signal transcription of the androgen receptor.The compound has good biological activity at the protein level, the cell level and the animal level, and has good safety.Therefore, the compound can be applied to the preparation of medicines for treating diseases such as tumors caused by abnormal expression of the androgen receptor, including but not limited to prostate cancer, breast cancer and ovarian cancer.

The invention belongs to the technical field of organic synthesis, and particularly discloses a method for synthesizing neroli through 4-methyl-4-[(3-methylbutyl-3-alkene-1-yl) oxy]-2-(2-methylpropyl-1-alkene-1-yl) oxacyclohexane. The method comprises the following steps: taking 4-methyl-4-[(3-methylbutyl-3-alkene-1-yl) oxy]-2-(2-methylpropyl-1-alkene-1-yl) oxacyclohexane as a raw material; comprising the following steps: uniformly mixing 4-methyl-4-[(3-methylbutyl-3-alkene-1-yl) oxy]-2-(2-methylpropyl-1-alkene-1-yl) oxacyclohexane with a solvent, preheating, pumping the mixture into a fixed bed reactor filled with a SO42-Fe2O3-La2O3 / SBA-15 solid acid catalyst at a certain flow rate, reacting for a period of time at a certain temperature and pressure, filtering, washing, and drying to obtain the 4-methyl-4-[(3-methylbutyl-3-alkene-1-yl) oxy]-2-(2-methylpropyl-1-alkene-1-yl) oxacyclohexane. After the reaction, cooling through a condenser to obtain a reaction crude product, and rectifying the crude product to obtain a neroli ether product and an isopentenol byproduct; the synthesis method disclosed by the invention is relatively mild in reaction condition, high in reaction speed and high in production efficiency, no wastewater is generated in reaction post-treatment, the solvent and the catalyst can be recycled for the next batch after being recycled, the production cost is greatly reduced, and industrial production is easy to realize. Meanwhile, by-products are utilized, and the production cost of nerolin is reduced.

The present disclosure provides a medical adhesive and a preparation method thereof, comprising a component A and a component B: the component A comprises a cycloketene acetal compound and an oxidizing agent; the component B comprises a vinyl monomer, a cross-linking agent and a reducing agent, wherein the cycloketene acetal compound is selected from one or more of 2-methylene-1,3-dioxepane, 2-methylene-4-phenyl-1,3-dioxolane, 5,6-benzo-2-methylene-1,3-dioxepane and 4,7-dimethyl-2-methylene-1,3-dioxepane. The medical adhesive overcomes the disadvantages of conventional medical adhesives.