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

The invention provides a crystal form of sorafenib tosylate, and a preparation method thereof. The X-ray powder diffraction pattern of sorafenib tosylate of crystal form B has diffraction peaks when the values of 2theta are about 7.34DEG, 18.03DEG, 20.15DEG, 20.77DEG, 22.04DEG, 22.43DEG and 23.21DEG; and the X-ray powder diffraction pattern of sorafenib tosylate of crystal form C has diffraction peaks when the values of 2theta are about 7.61DEG and 13-33DEG. The sorafenib tosylate of crystal form C is prepared through reduced pressure heating of the sorafenib tosylate of crystal form B. The invention also provides a preparation method of amorphous crystals of sorafenib tosylate through reduced pressure heating of the sorafenib tosylate of crystal form B or C. The sorafenib tosylate crystals prepared in the invention have the advantages of good stability, high crystallization purity, simple preparation process, and suitableness for industrial production.

The invention relates to the technical field of preparation of ceramic glazed bricks, and provides a wear-resistant antifouling ceramic starlight glazed brick and a preparation method thereof. The glittering effect is achieved through multiple reflection, dispersion and refraction methods of crystals in the glaze, a glaze layer of the glazed brick has the multi-layer glittering effect and the three-dimensional decoration effect, and the grade and decoration of the product are improved; and an excellent flashing effect can be achieved only by polishing according to a conventional polishing process of a glazed product. The glazed brick disclosed by the invention has relatively high hardness and excellent antifouling property and wear resistance.

The invention discloses a layered nanosheet ferrierite molecular sieve. The nanosheet ferrierite molecular sieve is characterized in that the molecular sieve is a high-crystallinity pure-phase ferrierite molecular sieve; the thickness of the sheet is between 30nm to 80nm; the specific surface area is larger than or equal to 340m<2>/g; the mesoporous surface area is larger than or equal to 60 m<2>/g; the crystallinity reaches 109% or more and is larger than or equal to 106%. The invention also relates to a preparation method of the layered nanosheet ferrierite molecular sieve and application ofthe layered nanosheet ferrierite molecular sieve to alkene oligomerization, low-density polyethylene cracking and skeleton isomerization reaction in n-butene and n-pentene.

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 provides crystals of an anilinopyrimidine compound with indole substituted by a trifluoroethyl group and salts thereof, wherein the anilinopyrimidine compound is used as an EGFR inhibitor. Specifically, the invention relates to a crystal of the compound as shown in a formula I which is described in the specification, a crystal of a monomesylate of the compound as shown in the formulaI or a dimesylate of the compound as shown in the formula I, and further relates to preparation methods for the crystals, crystal compositions containing the crystals, and pharmaceutical compositionscontaining the crystals or the crystal compositions and medical application thereof. The crystals provided by the invention have the advantages of high purity, high crystallization degree, good stability, etc.

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 invention relates to a chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide or its salt and a preparation method thereof. The chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide is an important intermediate for preparing a hepatitis C-resistant drug Telaprevir. The preparation method utilizes D-tartaric acid as a resolving agent to resolve 3-amino-N-cyclopropyl-2-hydroxyalkanamide so that the chiral intermediate (S, S)-3-amino-N-cyclopropyl-2-hydroxyalkanamide or its salt is obtained.

The invention relates to an m-aminobenzoic acid spherical crystal and a preparation method thereof. The method comprises the following steps: dissolving m-aminobenzoic acid I crystal form raw materials in an organic solvent at 45-65 DEG C under the stirring action to prepare an m-aminobenzoic acid solution, cooling the solution to 5-20 DEG C, continuously stirring until crystals emerge, continuously stirring for 30-60 minutes to coalesce the crystals into balls, separating solid and liquid crystal slurry, filtering, washing and drying a wet solid product to obtain m-aminobenzoic acid sphericalcrystals. The spherical crystal prepared by the invention can effectively improve the chemical stability and the crystal form stability of the m-aminobenzoic acid I crystal form. The purity of the spherical crystals is greater than 98%, the volume average particle size is 0.55-1.50 mm, the crystal particles are round, the fluidity is high, the repose angle is 24.3-27.7 degrees, the caking rate is3.0-6.5%, the tap density is 0.28-0.35 g/cm<3>, and the specific surface area is 0.14-0.23 m<2>/g.

The invention belongs to the technical field of pharmaceutical chemicals, and particularly discloses a refining method of aspirin-lysine. The refining method comprises the following steps: dissolving aspirin-DL-lysine in an ethanol water solution, adding absolute ethyl alcohol, cooling and crystallizing to prepare a refined aspirin-DL-lysine product. Experiments show that the content of free salicylic acid is greatly reduced after the aspirin-lysine is refined, so that the problem that the content of the free salicylic acid in the aspirin-lysine is relatively high due to sudden abnormal production conditions or improper storage conditions can be effectively solved. The method disclosed by the invention is simple in process, mild in crystallization condition, easy to control and low in cost, and has relatively high industrial application value.

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 belongs to the field of medicines, and particularly relates to a preparation method of mycophenolate sodium. According to the invention, mycophenolic acid is used as a raw material to prepare an M2 crystal form mycophenolate sodium bulk drug suitable for a preparation. According to the preparation method of the mycophenolate sodium, mycophenolic acids with various purities are used as raw materials and can be commercially purchased, and the raw materials are easy to obtain; according to the method, methyl isobutyl ketone which is low in toxicity is adopted as a solvent and is easy to recycle, the production cost is low, meanwhile, methyl isobutyl ketone serves as a crystallization solvent, the crystallization condition is mild, the obtained mycophenolate sodium is in an M2 crystal form, the stacking density ranges from 0.3 g/mL to 0.5 g/mL, and use of pharmaceutical preparations is facilitated. According to the preparation method of the mycophenolate sodium, the crystallization yield reaches up to 93% or above, the process is simple, and industrial production is facilitated.