31 results about "BEPOTASTINE BESILATE" patented technology

The present invention relates to an improved preparation method of bepotastine bepotastine, which comprises the following steps: the first step, combining 2-[(4-chlorophenyl)(4-piperidinyloxy)methyl]pyridine with Resolving agent reaction, obtain S-2-[(4-chlorophenyl) (4-piperidinyloxy) methyl] pyridine N-acetyl-L-phenylalanine salt, the second step, S ‑2‑[(4‑chlorophenyl) (4‑piperidinyloxy) methyl] pyridine N‑acetyl‑L‑phenylalanine salt plus acid extraction to obtain S‑2‑[(4‑chlorobenzene Base) (4-piperidinyloxy)methyl]pyridine, the third step, S-2-[(4-chlorophenyl)(4-piperidinyloxy)methyl]pyridine sequentially in acetonitrile Coupling reaction with ethyl 4-bromobutyrate, hydrolysis reaction and salt-forming reaction to obtain bepotastine besilate. The technical scheme of the invention greatly improves the yield, shortens the process time, and the obtained product has high purity, safety and stability.

The invention relates to a bepotastine besilate tablet and a preparation method thereof, and belongs to the technical field of medicament. The bepotastine besilate tablet is mainly prepared from the following components in parts by weight: 5 to 10 parts of bepotastine besilate, 50 to 90 parts of mannitol, 6 to 12 parts of PEG (Polyethylene Glycol) 6000, 0.2 to 2 parts of hydroxypropyl methyl cellulose, 5 to 10 parts of microcrystalline cellulose and 1 to 3 parts of magnesium stearate. The preparation method is characterized by during a preparation process, firstly, mixing active components, afilling agent and an adhesive, and then adding an adhesive solution prepared from the adhesive and water, thus preparing a soft material; secondly, pelleting; finally, carrying out tabletting and coating on granules with an anti-adhesion agent and a lubricating agent. A preparation technology comprises the following steps of pretreatment of auxiliary materials, mixing, wet granulation, drying, grain finishing, total mixing, tabletting and coating. The bepotastine besilate tablet prepared by adopting the preparation method has good dissolubility and is stable in quality, simple in preparation technology and suitable for large-scale production.

The invention discloses a bepotastine besilate nasal spray and a preparation method thereof. For the nasal spray, 1-10 g of bepotastine besilate and 3-15 g of solubilizing composition are added in 100 mL of water; the solubilizing composition comprises components in percentage by weight as follows: 80%-95% of propylene glycol, polyethylene glycol 300 or polyethylene glycol 400 and the balance of caprylocaproyl macrogolglycerides; and pH of a nasal spray solution ranges from 6 to 8. In the composition, bepotastine besilate does not exist in a solid particle mode and cannot be crystallized during a long-term storage process, so that not only is rapid medicine absorption facilitated, but also a spray pump port is not blocked easily, and anaphylactic rhinitis and mucous membrane inflammation related to rhinitis can be cured effectively.

The invention relates to an asymmetric synthesis method of an ophthalmologic drug pylistramine besylate. The method concretely comprises the following steps: oxidizing (4-chlorophenyl)(2-pyridyl)methanone to obtain (4-chlorophenyl)(2-pyridyl)ketone-N-oxide; carrying out asymmetric transfer hydrogenation reduction on the (4-chlorophenyl)(2-pyridyl)ketone-N-oxide through using a complex of monosulfonyl chiral diamine and metallic ruthenium, rhodium and iridium as a catalyst and a sodium formate or formic acid and triethylamine mixture or isopropanol as a hydrogen source in order to prepare (S)-(4-chlorophenyl)(2-pyridyl)methanol-N-oxide; reducing the (S)-(4-chlorophenyl)(2-pyridyl)methanol-N-oxide to prepare (S)-(4-chlorophenyl)(2-pyridyl)methanol; and condensing the (S)-(4-chlorophenyl)(2-pyridyl)methanol and ethyl 4-(4-bromopiperidine-1-yl)butyrate to obtain the ophthalmologic drug pylistramine besylate. The total yield is 61.6%.

The invention discloses a stable bepotastine besilate crystal in novel crystal form through a recrystallization method. The obtained bepotastine besilate crystal is confirmed through X-ray powder diffraction and infrared spectrum. Stability contrast experiments prove that the provided bepotastine besilate crystal has extremely high stability, and both bulk drug and preparation of the bepotastine besilate crystal have stability obviously better than that of existing bepotastine besilate crystals.

A method for splitting a Bepotastine Besilate optical isomer and quantitatively measuring R-isomer impurity is disclosed. According to the invention, high performance liquid chromatography is adopted. A mobile phase contains n-hexane and ethanol. The method is characterized in that normal-phase liquid chromatography is adopted; packing used in a chromatographic column is silica gel with its surface coated with amylase-tris-(3,5-xylyl carbamate); and the mobile phase also contains an alkaline additive. In comparison with the prior art, the method provided by the invention has advantages as follows: the mobile phase is simple to prepare, and resolutions of two isomers are both within 4.5-5.5. Especially, the chromatographic column of the method has good durability, and the chromatographic column still has high column efficiency after having been used for one year. Thus, analytic determination cost is greatly reduced.

The invention belongs to the field of analytical chemistry, in particular to a method for separating and measuring bepotastine besilate and potential genotoxic impurities thereof with a HPLC (High Performance Liquid Chromatography) method. According to the method, an adopted chromatographic column is characterized in that octadecylsilane chemically bonded silica is taken as a filler, a flowing phase A and a flowing phase B are adopted for performing gradient elution, and enter a detector for detecting; the potential genotoxic impurities includes ethyl benzenesulfonate and isopropyl benz-enesulfonate; the flowing phase A is a phosphoric acid solution, and the flowing phase B is an acidic acetonitrile solution. By adopting the method, the contents of the bepotastine besilate and the potential genotoxic impurities thereof can be effectively separated and measured; high sensitivity, specificity and repeatability are achieved; the measurement is not interfered by a solvent peak during detection, and a detection result is accurate and reliable, so that the method has an extremely important significance in realizing quality control for the bepotastine besilate and a preparation thereof.

The invention discloses a refining method for high-purity bepotastine besilate. The refining method is a solvent crystallization method adopting a crude bepotastine besilate product as a raw material and comprises the following steps: firstly, the crude bepotastine besilate product is heated and dissolved with acetonitrile and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and primary refined product is obtained; the primary refined product is heated, stirred, dissolved in water and filtered, a filtrate is cooled, stirred and crystallized, crystals are filtered and dried, and a pure bepotastine besilate product is obtained. The method has the advantages that the operation is simple and convenient, the yield is high, the product is pure, the cost is saved and the like, the total yield is 80% or higher, the purity of the pure bepotastine besilate product is 99.9% or higher proved by HPLC detection, the isomer impurity content is reduced to 0.1% or lower from 0.4%, and other single impurity content is reduced to 0.1% or lower from 0.2%.