42results about "Organic chemistry methods" patented technology

The invention relates to cariprazine tartrate (I), a crystal form, a preparation method therefor and use of cariprazine tartrate for treating schizophrenia and dual-phase type I disorder drugs. The compound provided by the invention is excellent in water solubility, flowability of powder and stability, and is an excellent medicinal form of cariprazine. The formula is shown in the description.

The invention provides a two-dimensional double perovskite material. The composition formula of the two-dimensional double perovskite material is AnMIIIMIX8, wherein A is organic amine; MIII is a trivalent metal element; MI is a monovalent metal element; and X is halogen. The two-dimensional double perovskite material has certain advantages of methylamine lead-iodine perovskite and lead-free double perovskite. The material is lead-free and environmentally friendly, has very good light stability and good chemical stability, and is unlikely to deteriorate in air. The material has a suitable andadjustable light absorption band gap, and more importantly can be used for preparing a film at a low temperature by a solution method. The advantages provide basis for the application of the materialin the photovoltaic fields such as solar cells, optical detectors and light-emitting diodes.

The invention discloses an agricultural amino acid composition. The bactericidal active component of the agricultural amino acid composition is L-pyroglutamic acid, and the L-pyroglutamic acid is separated from an extract of disporopsis aspera. The agricultural amino acid composition can be prepared into agriculturally acceptable soluble powder. The invention further discloses application of the agricultural amino acid composition to control of crop diseases. The agricultural amino acid composition has a relatively good preventive effect on cucumber downy mildew, potato late blight and grape downy mildew and has protecting and treating effects.

The invention relates to a preparation method of D-p-hydroxyphenylglycine methyl ester. The preparation method comprises the following steps: (1) esterifying: carrying out an esterification reaction on D-p-hydroxyphenylglycine and methanol to obtain D-p-hydroxyphenylglycine methyl ester sulfate, and distilling off methanol and water under reduced pressure, wherein the D-p-hydroxyphenylglycine is added one time, and the methanol is added in batches; and (2) crystallizing the D-p-hydroxyphenylglycine methyl ester. The preparation method can very easily control the reaction endpoint, so that theyield and the quality index of the finished product can be guaranteed to the maximum extent; the preparation method provided by the invention avoids the problems of safety and operation caused by hydrogen chloride gas or thionyl chloride; and in the step of D-p-hydroxyphenylglycine methyl ester crystallization, an alkali metal hydroxide is used for adjusting the pH value of the system without using ammonia water, so that the problem that ammonia ions are difficult to treat is avoided.

The invention relates to a method for manufacturing a sorbitol syrup having a total reducing sugar content no higher than 0.2% and mannitol content of less than 1%, with 70 wt % of dry matter. Said manufacturing method is characterized in that it includes the steps of: (a) hydrolyzing a solution of sucrose in a solution of invert sugars, (b) separating the solution of invert sugar by simulated moving bed chromatography into, on the one hand, a dextrose syrup having at least 99.3%, preferably 99.4%, more preferably at least 99.5%, and even more preferably 99.7% of dextrose content and, on the other hand, a fructose syrup having at least 90%, preferably 92% of fructose content, and (c) hydrogenating said dextrose syrup into a sorbitol syrup having a reducing sugar content no higher than 0.2% and a mannitol content of less than 1%, with 70 wt % of dry matter.

The invention discloses a preparation method of (2S,3S)-2,3-butanediol, and belongs to the technical field of biochemistry. The preparation method comprises the following steps of: stirring and mixingsolution containing ketoreductase with buffer solution to obtain mixed solution; in the stirring process, adding nicotinamide adenine dinucleotide, isopropanol and 2,3-butanedione into the mixed solution to perform closed reaction, so that reaction solution is obtained; carrying out reduced pressure suction filtration and rotary evaporation treatment on the reaction solution to obtain extractingsolution; and carrying out rectification separation on the extracting solution to obtain the (2S,3S)-2,3-butanediol. Meanwhile, the invention provides an amino acid sequence of the ketoreductase for catalyzing 2,3-butanedione to generate the (2S,3S)-2,3-butanediol. The invention further provides a nucleotide sequence for coding the ketoreductase. The preparation method is simple in synthetic routeand high in efficiency; 2,3-butanedione is reduced into (2S,3S)-2,3-butanediol by selecting the ketoreductase in an isopropanol system; the conversion rate of 2,3-butanedione can reach up to 95%; andin addition, the chiral purity of the prepared (2S,3S)-2,3-butanediol product can also reach 98%.

The invention relates to a metal organic complex containing a thiophene functional group and a preparing method and application of the metal organic complex. According to the technical scheme, Cd(NO3)2.6H2O, a ligand 2,2'-bithiophene-5,5'-dicarboxylic acid(H2btdc), a solvent N,N-dimethyl formamide and ethyl alcohol are added into a high-temperature-resistant spiral opening glass bottle, and stirring is carried out at the room temperature; the container is sealed and then put into an oven, and heating is carried out for 1-2 days at the temperature of 75 DEG C; the container is slowly cooled to the room temperature, and yellow transparent bulk crystals are obtained; the mixture is washed with N,N-dimethyl formamide, filtered and dried, and the target product is obtained. The prepared metal organic complex containing the thiophene functional group shows a good fluorescence characteristic and can be used for efficiently and selectively recognizing heavy metal zinc ions.

The invention discloses a salt of 5-fluorouracil and metformin as well as a preparation method and a crystal structure of the salt and relates to the field of medicinal chemistry. The molecular formula of the 5-fluorouracil metformin salt is C8H14FN7O2; and a basic structural unit is formed by a metformin anion and a 5-fluorouracil anion. The salt belongs to a monoclinic crystal system with a space group of P21/n. The preparation method comprises the following steps: taking a 5-fluorouracil crude drug and metformin free alkali as raw materials; mixing the 5-fluorouracil crude drug and the metformin free alkali according to the molar ratio of 1 to 1 and dissolving a mixture into a mixed solvent of methanol and acetonitrile for reacting; and taking ethanol as a solvent and recrystallizing toobtain high-purity 5-fluorouracil metformin salt. The 5-fluorouracil metformin salt disclosed by the invention has the advantages that the solubility of the 5-fluorouracil is improved and bioavailability of the 5-fluorouracil is favorably improved. The salt structure has no crystallized solvent molecules, so that a framework structure of the crystal of the salt can be kept after the salt is stored under the condition of room temperature for a long term and no denaturation phenomenon is caused.

Compounds having activity as inhibitors of G12C mutant KRAS protein are provided. The compounds have the following structure (I): or a pharmaceutically acceptable salt, stereoisomer, isotopic form or prodrug thereof, wherein R¹, L¹, L², L³, A¹, A², A³, A⁴, G¹, G², E, W, X, Y, Z, m, and n are as defined herein. Methods associated with preparation and use of such compounds, pharmaceutical compositions comprising such compounds and methods to modulate the activity of G12C mutant KRAS protein for treatment of disorders, such as cancer, are also provided.

The invention provides two new crystal forms: a crystal form E and a crystal form F, of canagliflozin, and the preparation method thereof. The new crystal forms are greatly improved in form and particle size. The particles are fine in size and are dispersed uniformly, so that it is beneficial to improvement of medicine solubility and dissolution rate, thereby being beneficial to preparation development.

Embodiments are provided that provide for efficient production of highly pure natural I-menthol. In some embodiments, a method for preparing natural I-menthol involves providing crude mentha oil in a crystallizer and gradually reducing the temperature of the crystallizer in a step-wise manner, thereby producing highly pure crystals in less than two weeks. The methods disclosed herein are suitable for pharmaceutical GMP.

The invention provides a method for preparation of tadalafil crystal form with two solvents. The method adopts dimethyl sulfoxide and water as the solvent, and compared with the current use of multiple mixed organic solvents, the method significantly reduces the variety and dosage of organic solvents, and reduces energy consumption compared with recrystallization. The process is completed at roomtemperature without heating and cooling, increases the productivity, lowers the production cost, and has remarkable economic value and environmental protection value.

The invention relates to a novel crystal form of nilotinib and belongs to the technical field of preparation of bulk drugs. The novel crystal form of nilotinib can produce characteristic peaks at diffraction angles of 6.76 degrees, 7.44 degrees, 12.86 degrees, 13.48 degrees, 16.71 degrees, 19.72 degrees, 21.85 degrees, 22.89 degrees, 25.98 degrees, 26.86 degrees and 29.24 degrees. The novel crystal form of nilotinib greatly improves the solubility of the bulk drug.

The invention disclose a chemical compound as shown in Formula I in the specification, wherein R1, R2 and R3 are selected from methyl, ethyl, propyl, butyl, amyl or hexyl. The invention further discloses a crystal form of the chemical compound, preparation methods and applications of the chemical compound and the crystal form. The chemical compound or the crystal form of the chemical compound has an inhibition effect on cell multiplication of a leukemia cell line MV4-11, and a new choice for screening a drug for treatment or prevention of leukemia in clinic is provided.

The invention provides a method for separating all-trans fatty acid with antitumor activity from antarctic krill oil. According to the method, the antarctic krill oil is subjected to silica-gel chromatography coupling, high-performance liquid chromatography is prepared to carry out separation and purification, antitumor activity detection is carried out in an assisting manner so as to determine effective ingredients, molecular weights, structural compositions and configurations of the effective ingredients are determined separately through high-resolution electro-spraying ionization mass spectrum, nuclear magnetic resonance and a laser Raman scattered spectrum, and the effective ingredients are identified as all-trans EPA and all-trans DHA. Discovered by comparison of median lethal concentration of antarctic krill, commercially-available deep-sea fish oil and Amur sturgeon fish liver EPA and DHA to a variety of tumor cells, the all-trans EPA and all-trans DHA originated from the antarctic krill oil have a good tumor cell growth resisting action and are free of obvious inhibiting effect on normal control cells, thereby having a potential antitumor candidate drug development prospect.

The present invention provides zuclomiphene salts, zuclomiphene binaphthyl hydrogen phosphate salt (1-A)⋅(BPA) and zuclomiphene oxalate salt (1-A)⋅(OXL), crystalline forms thereof and processes for the preparation thereof.

The invention discloses a quinolizine aza-bis-aromatic ring axial chiral compound and a synthesis method of the quinolizine aza-bis-aromatic ring axial chiral compound. The method comprises the following steps: firstly obtaining an intermediate from raw materials substituted 1-naphthyne and methyl chloroformate under the action of lithium diisopropylamide, then generating a precursor from the intermediate and 2-methylpyridine under the action of lithium diisopropylamide, and finally reacting the precursor under the action of CuCl and a chiral phosphamide ligand to obtain the quinolizine aza-bis aromatic ring axial chiral compound. The method disclosed by the invention is mild in reaction condition and extremely high in yield and enantioselectivity, the quinolizine aza-bis-aromatic ring axial chiral compound taking quinolizine as a matrix is synthesized for the first time, and the range of the aza-axial chiral compound is greatly expanded.

This invention discloses a novel method for the conversion of carboxylic acids to carbothioic acids and application of the method to the preparation of androstane carbothiolates, such as fluticasone propionate, which avoids column chromatography.

The invention belongs to the field of medicines and relates to a cefmetazole crystal-form compound and a preparation method thereof. The cefmetazole crystal-form compound and the preparation method thereof, provided by the invention, are used for improving the quality stability of cefmetazole and safety in clinical medication. Shown by parameters such as melting point, IR and PXRD, the cefmetazole crystal-form compound is different from any novel crystal form in the prior art; compared with the existing cefmetazole on the market, the crystal-form compound has the advantages that the content of related substances is extremely low, the stability is high, and the content of related impurities is free of obvious increase along with the prolongation of storage time, so that the cefmetazole crystal-form compound is suitable for serving as a standard in detection analysis or quality control.

The invention relates to a synthesis method of guanine-based pearlescent pigment. The method comprises the following steps: 1) preparing a sodium salt or potassium salt solution of guanine by utilizing guanine and sodium hydroxide or potassium hydroxide; 2) preparing a dispersion liquid from formamide, a small molecular additive and a polymeric additive; and 3) adding the sodium salt or potassiumsalt solution of guanine into the dispersion liquid, mixing, standing and reacting for a certain period of time to obtain a dispersion liquid of guanine micro-sheets, and further obtaining the guaninemicro-sheets. By adopting the method disclosed by the invention, the guanine crystal micro-sheets with a specific exposed surface can be artificially synthesized, the guanine crystal micro-sheets have a size which can be compared with that of a biological extraction sample and have good water or other solvent dispersibility, and the dispersion liquid has an obvious pearlescent color.

The present disclosure is generally directed to methods for purifying cannabinoids from Cannabis plants.

The present invention relates to process for the preparation of Empagliflozin or its co-crystals, solvates and/or polymorphs thereof. The present invention also relates to novel intermediates used therein, and process for the preparation thereof. The present invention further relates to process for preparation of amorphous and crystalline form of Empagliflozin.

The invention relates to a two-dimensional layered germanium-vanadium-oxygen cluster compound and a synthesis method and application thereof.The chemical formula of the germanium-vanadium-oxygen cluster compound is [Zn (en) (H2O)] 4 [Zn (en) 2] 2 [Ge6V15O48]. 4.5 H2O. The preparation method of the germanium-vanadium-oxygen cluster compound comprises the steps that NH4VO3, GeO2, Zn (Ac) 2.2 H2O, terephthalic acid and 1, 2, 4-triazole are put into a polytetrafluoroethylene lining, then ethylenediamine and H2O are added, stirring is conducted for 20-35 min, and a mixed solution is obtained; and the mixed solution is placed in an oven at 140-180 DEG C to react for 3-6 days, cooling to room temperature, washing with distilled water, and filtering are carried out to obtain brown flaky crystals, namely the two-dimensional layered germanium-vanadium-oxygen cluster compound. The germanium-vanadium-oxygen cluster compound has antiferromagnetism, is a potential magnetic storage material, and can be applied to preparation of some magnetic materials.