1996results about "Carboxylic acid amide separation/purification" patented technology

The crystalline form V of a compound of formula (I) is characterised by the X diffraction diagram thereof on a powder.

The crystalline form IV of a compound of formula (I) is characterised by the X diffraction diagram thereof on a powder.

The crystalline form III of a compound of formula (I) is characterised by the X diffraction diagram thereof on a powder, and the drugs contains it.

The invention discloses a preparation method of one of components of a novel antihypertensive drug LCZ696, namely, sacubitril (sacubitril, AHU-377, I). The method comprises the following preparation steps: carrying out cyclization, addition, debenzylation, ring opening, esterification, amidation and the like on a chiral induciton reagent (S)-1-(alpha-aminobenzyl)-2-naphthol (S-betti Base) and 2R-methyl-4-oxo-butyric acid to prepare the sacubitril (I). The preparation method is available in raw materials, concise in process, economic and environmentally friendly, and is suitable for industrial production.

The invention discloses an extracting polyphenol, theanine, tea polysaccharide and tea pigment method from tea, which is characterized by the following: using deionized water for lixiviating tea at constant temperature with continuous flow upstream at multi-speed; adopting microstrainer to dislodge the foreign matter of raffinate; using hyperfiltration for putting-off pectin and protein; concentrating by hyperfiltration and dehydration; extracting tea polyphenol by acetic acid ethyl ester and recovering dissolvant; stripping caffeine of extracting extract phase, pesticide residue and dissolvant by CO2 supercritical fluid; getting tea polyphenol by low-temperature nitrogen spray-drying; using alcohol separation and low temperation vacuum drying by hyperfiltration trapped fluid to prepare tea polysaccharide; separating alcohol recrystallization by basic copper carbonate and hydrogen sulfide to get theanine; using enzymatic oxidation and alkaline air to oxygenate remain polyphenols substance of liquid phantom; getting tea pigment by hyperfiltration dehydration compression and vacuum drying; merging caffeine form carbon dioxide above-critical fluid and caffeine from carrene; recovering dissolvent; using deionized water for washing; obtaining caffeine by recrystallization vacuum drying.

The invention discloses a preparation method of an agomelatine I type crystal which is an anti-depressant. The preparation method comprises the following steps of: dissolving crude agomelatine in a hydrophily organic solvent, filtering, dropping the filtrate into water under stirring, separating out solids and drying; wherein the weight part ratio of the hydrophily organic solvent to the water is 1:2-50. The agomelatine I type crystal prepared by the invention has excellent quality, good reproducibility, and high purity of HPLC normalization method to be above 99 percent, and is more suitable for large-scale industrialization production.

The present invention discloses a novel crystalline form of an angiotensin receptor antagonist and neutral endopeptidase inhibitor supramolecular complex. The novel crystalline form of the supramolecular complex has high water solubility and good stability. Experiments show that the moisture absorption and intrinsic dissolution extent and speed are superior to those of a conventional crystalline supramolecular complex.

The invention relates to a preparation method of a pharmaceutical compound and particularly relates to a method for preparing a cardiotonic drug LCZ696. Particularly the synthetic route of the compound is as shown in the specification.

The invention discloses a medicine of Agomelatine for treating depression, in particular an Agomelatine crystal and a medicine composition thereof. The Agomelatine crystal is irradiated by using Cu-K alpha; and an X-ray powder diffraction spectrum expressed by the degree of 2theta of the Agomelatine crystal has characteristic diffraction peaks at positions of 12.84, 13.84, 16.14, 14.18, 18.56, 19.12, 20.86, 21.20 and 23.84, and an infrared absorption spectrum of the Agomelatine crystal has characteristic diffraction peaks approximately at position of 3234, 3060, 2940, 1638, 1511, 1436, 1249, 1215, 1184, 1032, 908, 828, 755 and 588cm-1. The DSP heat absorption transition is 97.6 DEG C. The invention further discloses application of the medicine composition containing the Agomelatine crystal as an active effective component to the preparation of medicines for treating the depression.

A process for producing a long chain N-acyl acidic amino acid removes impurities by separating a mixture composed of a long chain N-acyl acidic amino acid containing an inorganic salt and a medium containing water and tertiary butanol into an aqueous layer and an organic layer containing the long chain N-acyl acidic amino acid at a temperature of from 35 to 80° C.

A water-soluble aspirin-theanine cocrystal composition which includes a quantity of acetylsalicylic acid and a quantity of a theanine enantiomer associated with the quantity of acetylsalicylic acid. The composition may be created by a method including the steps of: (i) providing a quantity of acetylsalicylic acid; (ii) adding a quantity of a theanine enantiomer to the quantity of acetylsalicylic acid to form a mixture comprising the quantity of acetylsalicylic acid and the enantiomer of theanine; (iii) wetting the mixture; and (iv) grinding the mixture for a length of time sufficient to produce a dried crystalline mass. The water-soluble cocrystal composition is suitable for intravenous administration, preferably to humans.

A method for recycling dimethyl formamide relates to a method for recovering dimethyl formamide from waste water by an all-subpressure operation method. The method includes the steps of utilizing conduction oil or low-pressure steam as a heat source, sequentially leading the waste water containing DMF to four subpressure operation towers, and performing subpressure concentration in the first tower and the second tower, subpressure fractionating in the third tower and deacidification in the fourth tower, thereby obtaining finished DMF and methanoic acid. Due to the great decrease of stable operating temperature, the recovery rate of the DMF can reach over 99 percent, and the rate of purity reaches 99.99 percent; the resolution ratio of the DMF and the back evaporation rate of the peracid DMF are obviously reduced, a methanoic acid decomposition tower is cancelled, almost no DMF contains peracid, repeated rectification is not needed, and energy sources are saved by over 10 percent; and meanwhile, the dimethylamine quantity generated by decomposition is little and is completely absorbed by a boiler screen dust collection system without emission.

The invention provides sacubitril derivatives and medicine compositions, preparation methods and application thereof and belongs to the fields of medicine compounds and preparation thereof. The sacubitril derivatives comprise sacubitril lithium salt, sacubitril kali salt, sacubitril magnesium salt, sacubitril calcium salt, sacubitril strontium salt, sacubitril zinc salt, sacubitril ferric salt, sacubitril ammonium salt, sacubitril diethylamine salt, sacubitril ethylenediamine salt, sacubitril piperazine salt, sacubitril N-(2-ethoxyl)-pyrrolidine salt, sacubitril choline salt, sacubitril cholamine salt, sacubitril diethanol amine salt, sacubitril triethanolamine salt, sacubitril tromethamine salt, sacubitril meglumine salt, sacubitril diisopropylamine salt, sacubitril tert-butylamine salt, sacubitril N, N'-bis-benzyl ethylenediamine salt, sacubitril L-lysine salt, sacubitril L-arginine salt or sacubitril L-histidine salt.

Purification process of iohexol comprising the treatment of said product with 1-methoxy-2-propanol either alone or mixed with other solvents.

The invention relates to a four-effect rectification system for synthesizing a leather dimethyl formamide solution by a wet method, and a recovery method. The four-effect rectification system comprises decompressing concentration towers, a normal-pressure rectification tower and a decompressing deacidification tower, wherein one decompressing concentration tower is added between two decompressing concentration towers in a three-effect rectification recovery system; the normal-pressure rectification tower adopts a filler tower. The process comprises the steps of feeding and preheating. By the concentration towers, the processes of one-stage decompressing concentration, two-stage decompressing concentration, three-stage decompressing concentration, normal-pressure rectification and decompressing deacidification are adopted, wherein the one-stage decompressing concentration tower, the two-stage decompressing concentration tower, the three-stage decompressing concentration tower, the normal-pressure rectification tower and the decompressing deacidification tower all adopt filler towers. The recovery technological procedure adopts a circulation process, and the generated heat energy is circularly used between the procedures of steaming at a tower top, heating by a tower kettle, feeding, preheating, condensing a finished product, preheating, rectifying and boiling again. Compared with a three-effect DMF recovery process which is widely applied at present, energy is at least saved by more than 20%; the purity of a recovered finished product DMF reaches 99.99%, the water content is below 200ppm, the acidity is below 20ppm, and the alkalinity is below 10ppm.

Disclosed herein are methods for the recovery of an organic acid, such as a heat stable lactic acid, from a feed stream which contains at least one of an organic acid amide, an organic acid ammonium salt, or an alkylamine-organic acid complex. The feed stream is mixed with at least one azeotroping agent. The azeotroping agent is a hydrocarbon capable of forming at least one azeotrope with the organic acid that is produced by the thermal decomposition of the amide, ammonium salt, or complex in the feed stream. Preferably the azeotrope is a heteroazeotrope. The mixture of the feed stream and the azeotroping agent is heated to produce a vapor stream. The azeotrope is a component of the vapor stream. The vapor stream can be condensed to a liquid stream, and the organic acid is recovered in the liquid stream that is produced. When the azeotrope is a heteroazeotrope, the vapor stream can be condensed into a liquid stream, which can be separated into a first phase and a second phase. The first phase contains the highest concentration of organic acid and the second phase contains azeotroping agent. The organic acid can be further purified and / or concentrated from the separated first phase or from the liquid stream.

The invention discloses a preparation method of an agomelatine I crystal form, which comprises the steps of: adding agomelatine into a mixed solvent of amide and water, heating for dissolving, then reducing the temperature and separating out crystals, and drying to obtain a solid. The agomelatine is dissolved in the heated mixed solvent of the amide and water, and separated out slowly in a cooled mixed solvent of the amide and water, and the high-purity I crystal form can be stably obtained. The method has the advantages of high purity of reaching above 99 percent of the single crystal form, simple operation and good repeatability, and the like and is suitable for industrialized production.

The invention discloses a quadruple-effect method for rectifying and recycling waste water containing DMF. The method comprises the steps as follows: utilization of heat of a deamination tower, a first-grade decompression rectifying tower discharging major cycle technology, normal-pressure rectifying tower gas-phase discharge to a deacidification tower and improvements and innovations on techniques such as up and down backflow of the deacidification tower and the like. According to the method, heat inside a system is fully used, the circulation volume of refrigerant recycled water is reduced, the consumption of a primary heat source is saved, the operation and running of the whole system is more stable and simpler, and the quality of a DMF finished product is easier to control. The technological process improvement method can be applied to a triple-effect DMF recycling system as well.

A triple-effect distillation and recovery method for wet synthetic leather dimethylformamide(DMF) solution includes: feeding, preheating, condensing and separating it by a concentration tower and a distillation tower to output it to complete the recovery process, in which, low-pressured steam is the heating media, using decompressed concentration for step I, atmospheric concentration for level II and vacuum distillation, the decompressed concentration processes in the packing tower, atmospheric concentration processes in the plate column, decompressed concentration processes in the combined packing and plate column. In the described cycle process, energy can be recycled between the steam in the top, heating at the bottom, feed preheating, preheating of finished condensation, distillation, reboilling processes.

A process for extracting theanine comprises the steps of chitosan rouging by flocculation, decolorizing by adsorption, adsorbing by cationic ion-exchange resin, ammonia eluation, decompression concentration, adsorbing and rouging by anion exchange resin, concentration alcohol depositing, and recrystallization. The process by the invention can effectively remove the impurity which influences the exchange adsorption function of the cationic ion-exchange resin.

The invention relates to a method for comprehensively extracting effective ingredients in tea. The method comprises the following steps of: with a faintly acidic water solution as a main extraction solvent and a certain amount of organic solvent as an auxiliary extraction solvent, carrying out step-by-step extraction on water extracts to obtain four effective ingredients, namely tea polyphenol, caffeine, tea polysaccharide and theanine; and meanwhile, extracting tea protein from tea residues by using an alkali dissolution and acid deposition method. According to the method, as water is used as the main solvent, the cost is low, the reactions are mild and active ingredients are favorably preserved; as a certain amount of organic solvent is used as the auxiliary extraction solvent, the problems of overhigh cost and product pollution caused by use of a large amount of organic solvents are solved; meanwhile, five effective ingredients, namely the tea polyphenol, the tea polysaccharide, the caffeine, the theanine and the tea protein are extracted, and therefore high extraction rate, high purity and high utilization rate of tea are achieved; the solvents are recycled in the extraction process, so that the preparation cost is reduced; and no alkali and acid waste liquor is discharged in the overall process, and therefore the method is environment-friendly. The overall preparation flow is high in efficiency and low in cost, and therefore the method has a favorable application value.

The present invention belongs to the field of medicine and health care article amino acid, and includes pre-treatment of the fermented liquid to eliminate thallus, partial protein, pigment and polysaccharide, controlling the pH value of the fermented liquid after pre-treatment; electrodialysis to eliminate inorganic salt and regulating pH value again; leading in processed OH type anionic exchangecolumn to adsorb impurities and separate glutamine; decoloring, vacuum concentration, isoelectric crystallization, washing coarse crystal in organic solvent and drying. The said process has low exchange resin consumption, no conversion of glutamine in strong acid and strong alkali environment, low production cost and high total glutamine extracting rate up to 70%, and is suitable for industrial production.

The invention provides a method for purifying iodixanol. The invention adopts a recrystallization method to purify crude iodixanol prepared from dipolymer of 5-acetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo isophthalamide, after several times of repeated purification, an iodixanol product qualified to Pharmacopoeia standards is obtained. The inventive purification method can be effectively used for purification of crude iodixanol prepared from dipolymer of 5-acetamido-N,N'-bis(2,3-dihydroxypropyl)-2,4,6-triiodo isophthalamide, and the used solvent has low cost, so as to remarkably reduce cost compared with the prior purification method. In addition, the inventive purification method is a non-chromatographic solvent purification method and can obtain iodixanol with high purity and high content after several times of repeated purification, so as to meet the industrial production requirements of iodixanol product, as well as Pharmacopoeia standards.

The invention relates to a purifying method of natural functional components and provides a method for preparing capsicine monomers. The method for preparing capsicine monomers comprises the following technical steps of extracting capsicum essential oil or capsicum powder by alcohol, separating and purifying macroporous absorbent resin, recrystallizing a monomer crude product, and the like. The method for preparing a capsicine monomer extracts three capsicine monomers from the capsicum essential oil or the capsicum powder, has simple technology and low production cost, does not use a harmful organic solvent in a production process and is easy to realize industrialized production. The purity of capsicine, dihydrocapsaicine and a falling dihydrocapsaicine monomer which are produced by the method is larger than 98 percent, and the yield of the capsicine, the dihydrocapsaicine and the falling dihydrocapsaicine monomer are larger than 85 percent. The method for preparing capsicine monomers lays a solid foundation for the wide application of high-purity capsicine monomers.

A process for enhancing theanine extraction from plant material through a series of extraction, adsorption and filtration steps. More specifically, disclosed is a process for isolating theanine from a plant material, which includes the steps of: a) contacting the plant material with a solvent to obtain an extract comprising theanine; b) contacting the theanine extract with an adsorbent to obtain a theanine-containing eluate; and c) subjecting the theanine eluate to a filtration step to obtain a theanine-rich extract.

A method for reacting alkanolamine with ester in the presence of a metal silicate compound and, optionally, a catalyst, to produce a hydroxyalkyl amide composition with a decreased level of alkanolamine and residual catalyst.

The process of separating and purifying natural theanine belongs to the field of deep tea processing technology. The present invention uses the industrial waste liquid from tea polyphenol production as material to produce natural theanine through the steps of ultrafiltering, macroporous resin decolorizing, cationic exchange resin adsorption, ammonia water elution, microcrystal cellulose column chromatography and anhydrous alcohol crystallization. The present invention has theanine product purity over 95 % and total theanine recovering rate over 60 %, and is environment friendly.

The present invention relates to a 2-hydroxyarylamide derivative or a pharmaceutically acceptable salt thereof, a preparation method thereof, and a pharmaceutical composition for preventing or treating cancer comprising the same as an active ingredient. The 2-hydroxyarylamide derivative prepared by the present invention is excellent in the inhibition of the activity of TMPRSS4 serine protease and the suppression of the infiltration of TMPRSS4-expressed cancer cells, and thus can be useful as a composition for preventing or treating cancer by inhibiting TMPRSS4 over-expressed in cancer cells, particularly, colorectal cancer, lung cancer, breast cancer, prostate cancer, ovarian cancer, pancreatic cancer, or stomach cancer cells.

The present invention provides a DMF recycling method with low recycling cost and high recycling rate. In the method, DMF is pumped to a DMF cooler from a waste liquid tank for preheating; then the preheated DMF waste liquid is pumped to a dewatering tower which is vacuumized by a vacuum motor to -0.078 plus or minus0.01 MPa to evaporate part of liquid water; the DMP waste liquid from the dewatering tower is pumped to a reboiler to be heated to 68 plus or minus3 DEG C and be further concentrated, thereby obtaining DMF waste liquid with the mass percentage concentration of 40-50%; next, the DMF waste liquid from the reboiler is pumped to a heater to be heated to 120 plus or minus5 DEG C; the waste liquid from the heater is pumped to a rectifying tower to evaporate and separate liquid water from the DMF recycling liquid; the DMF recycling liquid from the rectifying tower is deacidified in a deacidification tower; and then the deacidified DMF recycling liquid is inspected through a sampling can, if qualified, the DMF recycling liquid is delivered to a DMF tank of finished products.