31results about How to "Mild conditions for crystallization" patented technology

The invention discloses a crystal form B of a tetrahydrothienopyridine compound with a structure as shown in a formula I, and a preparation method, a composition and application thereof. The inventionaims to solve the problems of many impurities, low content, poor crystal form stability and incapability of forming a medicine in the prior art. When the crystal form B is subjected to Cu-K alpha radiation, in an X-ray powder diffraction pattern expressed by a 2theta angle, characteristic peaks occur at 11.21 + / - 0.2 degrees, 12.61 + / - 0.2 degrees, 14.69 + / - 0.2 degrees, 16.14 + / - 0.2 degrees, 17.81 + / - 0.2 degrees, 20.22 + / - 0.2 degrees and 22.10 + / - 0.2 degrees. The crystal form B provided by the invention has the advantages of few impurities, good stability, good crystallinity and reproducibility, and is suitable for industrial production; and unexpected stronger ADP-induced platelet aggregation resistance and better flowability are also achieved.

The invention relates to a cobalt-containing modified aluminophosphate molecular sieve smoke adsorbing material as well as a preparation method and application thereof, belonging to the technical field of cigarettes. The preparation method of the material comprises the following processing steps of preparation, crystallization, drying and calcination of CoAPO-11 initial gel; preparing the cobalt-containing modified aluminophosphate molecular sieve smoke adsorbing material which is excellent in crystallization; adding the prepared material in the middle of a cigarette filter, and testing the smoke absorbing effect of the material. The result indicates that the material has an excellent adsorbing effect on hydrogen cyanide and crotonaldehyde. According to the preparation method provided by the invention, the raw materials are low in cost, the crystallization condition is relatively mild, and the energy consumption is low. The prepared material can be used for effectively reducing the release amount of the hydrogen cyanide and the crotonaldehyde in the smoke after lowering the cigarette filter, and the harm reduction effect is outstanding.

The invention discloses a crystal transformation method of aluminum hydride. The crystal transformation method of the aluminum hydride comprises the following steps: adding the aluminum hydride into a solvent under the atmosphere of dry nitrogen, stirring, performing suction filtration and removing insoluble impurities to obtain an aluminum hydride solution; performing ultrasonic treatment; performing rotary evaporation to obtain aluminum hydride solid granules; putting the aluminum hydride solid granules into the air, dissolving, filtering, performing rotary evaporation and vacuum-drying the product. According to the crystal transformation method of the aluminum hydride, the aluminum hydride, which exists in beta and gamma crystal forms, in the aluminum hydride is converted into alpha-aluminum hydride with higher stability, and the impurity aluminum and the rest aluminum hydride which exist in an unstable crystal form are removed from the aluminum hydride. The crystal transformation method provided by the invention is high in crystal transformation efficiency, mild in crystal transformation condition and easy to operate and control. The purity of the alpha-aluminum hydride obtained after crystal transformation can reach above 99 percent, and the alpha-aluminum hydride can exist stably in the air atmosphere.

The application belongs to the field of medicinal chemistry, and relates to the crystallization of a trifluoroethyl-substituted indole aniline pyrimidine compound and its salt as an EGFR inhibitor. Specifically, the application relates to the crystallization of the compound represented by formula I, the Monomethanesulfonate crystals of the compound represented by formula I or dimesylate crystals of the compound represented by formula I also relate to a preparation method for the crystals, a crystal composition containing the crystals, a pharmaceutical composition containing the crystals or a crystal composition thereof and their medicinal uses. The crystal of the present application has the advantages of high purity, high crystallinity, good stability and the like.

The invention relates to the field of medicines, and discloses a crystal of tenofovir alafenamide hemifumarate and a preparation method thereof. The X-ray powder diffraction of the crystal has characteristic peaks at the following 2 theta angle positions: 7.02 degrees, 8.62 degrees, 11.02 degrees, 12.12 degrees, 13.90 degrees, 15.86 degrees, 16.30 degrees, 17.62 degrees, 18.32 degrees, 20.26 degrees, 20.82 degrees, 23.16 degrees, 26.60 degrees and 27.84 degrees. The tenofovir alafenamide hemifumarate crystal prepared by the invention has the advantages of good fluidity, low moisture absorption and stable crystal form, and is especially suitable for pharmaceutical preparations.

The invention discloses a crystal form of pralatrexate, a pharmaceutical composition containing the pralatrexate, and a preparation method and an application of the pralatrexate. According to the crystal form, in an X-ray powder diffraction pattern using a radiation source as Cu-Kalpha, characteristic absorption peaks are formed at the diffraction angles 2theta of 8.29 degrees, 15.73 degrees, 16.72 degrees, 17.21 degrees, 18.46 degrees, 19.01 degrees, 21.38 degrees, 25.25 degrees and 25.56 degrees; and the error range of 2theta is + / -0.2 degrees. The preparation method of the crystal form disclosed by the invention comprises the following steps: heating and dissolving pralatrexate into a good solvent; and dropwise adding an anti-solvent until turbidity is achieved, naturally cooling, and devitrifying, so as to obtain the crystal form. The crystal form of the pralatrexate disclosed by the invention has the advantages of high purity, good stability and the like.

The invention relates to a spherical crystal of m-aminobenzoic acid and a preparation method thereof. Under stirring at 45~65 ℃, the raw material of m-aminobenzoic acid crystal form I was dissolved in an organic solvent to prepare a m-aminobenzoic acid solution, the solution was cooled to 5~20 ℃, and the stirring was continued until the crystals appeared, and the stirring was continued for 30 minutes. ~60min, the crystals are coalesced into balls, then the solid liquid crystal slurry is separated, and the wet solid product is filtered, washed and dried to obtain m-aminobenzoic acid spherical crystals. The spherical crystal prepared by the invention can effectively improve the chemical stability and crystal stability of the crystal form I of m-aminobenzoic acid. The purity of spherical crystals is more than 98%, the volume average particle size is 0.55-1.50mm, the crystal particles are round, the fluidity is high, the angle of repose is 24.3-27.7°, the agglomeration rate is 3.0-6.5%, and the tap density is 0.28-0.35g / cm3, the specific surface area is 0.14 ~ 0.23m2 / g.

The invention provides a tenofovir preparation method suitable for industrialized production. According to the method, tenofovir is obtained through catalyzing and hydrolyzing a raw material intermediate (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine via trimethylbromosilane, wherein the raw material intermediate (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine is obtained through the following steps: firstly, obtaining (R)-9-(2-hydroxypropyl)adenine via the ring-opening condensation of adenine and (R)-epoxypropane under an alkaline condition; secondly, catalyzing the (R)-9-(2-hydroxypropyl)adenine through lithium t-butoxide; thirdly, conducting etherification on the catalyzed (R)-9-(2-hydroxypropyl)adenine and p-benzenesulfonyloxymethyl phosphoric acid diethylester, so as to obtain the (R)-9-[2-(diethylphosphonomethoxy)propyl]adenine. The method is characterized in that purified water of appropriate proportion is added in a mixed product obtained through catalyzing and hydrolyzing the (R)-9-[2-(diethylphosphonomethoxy)propyl] adenine via trimethylbromosilane; the tenofovir is obtained through spontaneous crystallization at an appropriate temperature and cooling rate, as well as at an appropriate stirring speed. According to the invention, the obtained tenofovir product has the characteristics of high yield, strong indissolubility in operation under room temperature, simplicity in filtration and collection due to large particles, short production time, low energy consumption, and the like.

The invention relates to azoxystrobin acetic acid solvate and a preparation method thereof. Its X-ray powder diffraction pattern is at diffraction angle 2θ=7.40±0.20°, 8.28±0.20°, 13.26±0.20°, 14.07±0.20°, 14.52±0.20°, 18.08±0.20°, 18.42±0.20°, 18.86±0.20 °, 20.46±0.20°, 21.18±0.20°, 22.14±0.20°, 22.68±0.20°, 24.46±0.20°, 26.88±0.20°, 28.60±0.20°, etc. have characteristic peaks, of which 7.40±0.20° is the starting point peak, the relative intensity of the characteristic peak at 21.18±0.20° is 100%. The preparation method is a constant-temperature suspension crystallization method, and the operation is simple, the reproducibility is good, the product has good fluidity, is not easy to coalesce, and is easy to be industrialized.

The invention relates to the field of medicinal chemistry and particularly relates to a new crystal form of the bortezomib. The invention additionally discloses a preparation of the crystal form and an application in the antineoplastic medicine. The crystal form disclosed by the invention solves the technical problems that the current bortezomib crystal form has bad solubility and weak antioxidant ability and is not good for liquid formulation preparation, and has the advantages of good solubility, high stability and strong antioxidant ability; simultaneously the crystal form prepared by the method disclosed by the invention is high in crystal form purity and safe in medicine use.

Steroid derivative FXR agonist (Formula I) crystal or amorphous substance, and preparation method thereof, crystal composition and pharmaceutical composition containing the crystal or amorphous substance, and their preparation for treating or preventing FXR related The purposes in the medicine of this kind of disease.

The invention discloses a preparation method of high-content geniposide crystals. The preparation method comprises the steps that cape jasmine fruits are smashed, extracted with ethyl alcohol, adsorbed with kieselguhr and then concentrated to obtain geniposide extracting extractum; extracting is performed with a mixed solution of ethyl acetate and methyl alcohol to obtain crude geniposide; the crude geniposide is dissolved with a methyl alcohol solution to obtain a saturated solution, cooling is performed after immediate filtration is performed, analytically pure ethyl acetate is added for first-time stirring crystallizing, solution adding is stopped, standing is performed for several hours, the analytically pure ethyl acetate is added for second-time stirring crystallizing until acicular crystals stop growing, a crystallizing system is obtained, and after filtering and reduced-pressure drying are performed, the snowy white acicular geniposide crystals are obtained. According to the crystals obtained through the method, it is detected that the geniposide purity can be more than 98.8 percent, and no toxic substance residue exists. The preparation method is mild in condition, low in cost and high in speed, has the advantages of being safe in production process, easy and convenient to operate, low in cost, short in cycle, high in product quality and stable in quality, and is suitable for industrialized production.

The invention provides a high-purity Pralatrexate solid and its preparation method. The high-purity Pralatrexate solid provided by the invention is prepared by recrystallization of an aqueous solution of lower alkyl ketone and has advantages of high purity, low individual impurity content, good stability, high safety and the like. Meanwhile, the preparation method of the high-purity Pralatrexate solid provided by the invention can be adopted to effectively remove IN0222(2,4-diamido-6-chloromethylpteridine) or its analogue and raise safety of medicine. In addition, the preparation method of the high-purity Pralatrexate solid is simple, a solvent is cheap and easily available, and crystallization condition is mild. The preparation method is suitable for industrial production.