31results about How to "Avoid chromatography" patented technology

The invention discloses a thermoshrinkable polyester film and a preparation method thereof. The preparation method comprises steps as follows: various polyester raw materials subjected to dust removal respectively enter storage bins, are respectively metered by an agravic weigher according to the proportion, simultaneously enter an inlet of a double screw extruder, are subjected to melt extrusion by a sandwich layer double screw extruder and two surface layer double screw extruders, and form a casting piece through a three-layer co-extrusion die head; the casting piece is respectively subjected to longitudinal stretching and lateral stretching, wherein the longitudinal stretching comprises a preheating zone, a stretching zone, a thermal setting zone and a cooling zone, and the thermal setting zone of the lateral stretching is more than 15m long; and the casting piece is subjected to traction rolling to obtain the thermoshrinkable polyester film. By adopting the proportioning mode of directly feeding after accurate metering by people, the instantaneous addition error range of various materials is at most 1%; and the material is biaxially stretched, so that the produced film has the advantages of greatly higher density, strength and uniformity, lower longitudinal shrinkage and lateral low-temperature shrinkage, and especially higher ductility and thermoshrinkable uniformity.

The invention discloses a method for synthesizing N-substitute-1, 2, 3, 6-tetrahydropyridine-5-boric acid ester. According to the method, N-substitute-1, 2, 3, 6-tetrahydropyridine-5-carboxylic acid (ester) serves as the raw material, conducts addition with halogen and then is subjected to alkaline condition elimination to form alkenyl halide and then subjected to coupling with al boron ester under the condition of metal palladium catalyzation, and the N-substitute-1, 2, 3, 6-tetrahydropyridine-5-boric acid ester is obtained. According to the method, the obtained midbody alkenyl halide does not contain isomer, separation is easy to conduct, purity of an obtained product is high, and the method provides a simple way for synthesis of compounds of the type.

The invention provides a preparation method of 3-methoxycarbonyl-6-methyl-4-(3-nitrophenyl)-2-formyl-1, 4-dihydropyridine-5-isopropyl carbonate. The method comprises the following steps that condensation and amination reactions between pyruvic aldehyde dimethyl acetal and dimethyl carbonate are carried out under the catalysis of a strong base to obtain 3-amino-4, 4-dimethoxyl-methyl crotonate; dehydration condensation reaction between isopropyl acetoacetate and nitrobenzaldehyde is carried out under the catalysis of a weak base to obtain 2-(3-nitrobenzylidene)-isopropyl acetoacetate; dehydration condensation and hydrolysis reactions between 3-amino-4, 4-dimethoxyl-methyl crotonate and 2-(3-nitrobenzylidene)-isopropyl acetoacetate are carried out to obtain 3-methoxycarbonyl-6-methyl-4-(3-nitrophenyl)-2-formyl-1, 4-dihydropyridine-5-isopropyl carbonate. The method provided by the invention solves the technical problems in the prior art including complex preparation process, low purity and less yield during the preparation of nilvadipine intermediate 3-methoxycarbonyl-6-methyl-4-(3-nitrophenyl)-2-formyl-1, 4-dihydropyridine-5-isopropyl carbonate.

The invention belongs to the technical field, and concretely relates to a method for preparing tribenoside. The method comprises the specific steps: 3,5,6-tribenzyloxy-1,2-oxygen-isopropylidene-alpha-D-furanose is taken as a starting reactant, a deprotection reaction is carried out under acidic conditions to generate a 3,5,6-tribenzyloxy-D-glucofuranose crude product, two-time refining purification is carried out to obtain a 3,5,6-tribenzyloxy-D-glucofuranose pure product, and finally, ethyl-3,5,6-tribenzyloxy-D-glucopyranoside is obtained by etherification under acidic conditions. The methodof is used for preparing the tribenoside, and intermediate synthesis, separation and purification processes are simple and convenient, which avoid column chromatography operation, and the final product has good quality and high purity, and the production cycle can be shortened obviously.

The invention relates to a method for preparing 1-hydroxy-3,5-dimethyl adamantine. The method comprises the steps as follows: (1) reacting 1,3-dimethyl adamantine and bromine at 40-100 DEG C for 0.25-10 hours with water being hydrolytic reaction reagent, and recovering bromine when the reaction is finished to obtain 1-bromo-3,5-dimethyl adamantine; and (2) reacting 1-bromo-3,5-dimethyl adamantine with water at 50-100 DEG C for 1-10 hours, cooling, vacuum filtering, water washing and collecting to obtain the target product. The obtained product has a yield of 95% or higher and a purity of more than 99.0%. Compared with the prior art, the method has the advantages that expensive chemical reagents and a silica gel column chromatography are not adopted, thus facilitating reducing production cost and improving yield.

The invention belongs to the technical field of medicine synthesis methods, and provides a preparation method of aripiprazole lauroxil. The preparation method comprises the following steps: (1) carrying out a hydroxymethylation reaction: contacting and reacting aripiprazole, an aqueous formaldehyde solution having a mass concentration of 35-40 wt% and an alkali in an organic solvent to obtain hydroxymethyl aripiprazole; and (2) carrying out a lauroylation reaction: contacting and reacting the hydroxymethyl aripiprazole, an organic alkali and lauroyl chloride in a solvent which is immiscible with water at 20-30 DEG C, and then recrystallizing the obtained reaction product in a crystallization solvent to obtain the aripiprazole lauroxil. The method of the invention can improve the yield of the two-step reaction of hydroxymethylation and lauroylation and the purity of the product, and also can shorten the reaction time, simplify the post-treatment process and reduce the material cost.

The invention provides a preparation method of enzalutamide. The method comprises the following steps: condensing an initial raw material 2-((3-fluoro-4-(methylcarbamoyl)phenyl)amino)-2-methylpropioric acid and enol to obtain an intermediate I, and reacting the intermediate I with The method has the advantages of simple operation, suitableness for industrial production, high yield and high purity.

The invention discloses a method for preparing a ticagrelor solution. According to the invention, hydroxy of a ticagrelor I crude product is protected by a protective group, then a crude product of a compound II is separated and purified to obtain the high purity compound II; the hydroxy protective group of the high purity compound II is removed under proper reaction conditions, a reaction mixture is post-processed and then the by-product is removed to obtain the high purity ticagrelor I, the ticagrelor I, a solvent or/and pharmaceutic adjuvant form a solution, after the solvent is removed, ticagrelor or a mixture containing ticagrelor and accessory with medicinal requirement can be obtained. The method has the advantages of mild reaction condition, simple operation, low cost, and environmental protection, and is suitable for industrial production.

The invention discloses a disturbance agitator for asphalt joint filling factice for a building. The disturbance agitator comprises an upright column, a base, a brake wheel, a heat-preservation tank body, a turbulence agitator and a friction plate, wherein the upright column is welded at the upper end of the base; the upper end of the upright column is provided with a revolving shaft; the brake wheel is welded at the end of the revolving shaft on the outer side of the upright column; the outer side of the brake wheel is provided with the friction plate; the friction plate is fixedly arranged on a brake frame; the brake frame is welded on a push rod of an electric push rod; a magnet is inlaid in the brake wheel; the outer side of the magnet is provided with an inductive probe. The disturbance agitator for the asphalt joint filling factice for the building is stale in structure, is firmly welded, is convenient for driving a rotating shaft of an agitating shaft; while a plurality of agitating rods on the turbulence agitator are used for agitating the mixed liquor of asphalt and oily slurry, the mixed liquor of the asphalt and the oily slurry flows out from a turbulence groove to form a plurality of interference flows; the mixing uniformity of the mixed liquor of the asphalt and the oily slurry is further enhanced; the generation of laminar precipitation or separation is avoided; the mixing sufficiency is guaranteed.

The invention discloses a refining method for improving optical purity of an eribulin intermediate compound. The refining method specifically comprises the following steps: (1) reacting a free compound (I) with sodium hydrogen sulfite to obtain a solid compound (II); and (2) recrystallizing the compound (II) and then dissociating into a compound (I). The reaction is a process of recrystallizationafter dissolution, column chromatography is avoided, and the method is safe, environmentally friendly, high in speed, clean in reaction process, free of redundant products, high in optical purity of products and suitable for large-scale production.

The invention discloses a refining method of fasudil hydrochloride. The method comprises the following steps: reacting homopiperazine with 5-isoquinoline sulfonyl chloride to obtain Fasudil free alkali, dissolving the Fasudil free alkali in a solvent A, uniformly mixing, dropwise adding hydrochloric acid into the solution at a constant temperature to adjust the pH value, stirring the solution at alow temperature to crystallize, filtering, drying a filter cake to constant weight to obtain Fasudil dihydrochloride, dissolving fasudil dihydrochloride in a solvent B, mixing, adding sodium hydroxide to adjust the pH value, separating the liquid, filtering the organic phase to obtain a filtrate, adding hydrochloric acid into the filtrate at constant temperature, stirring to crystallize, filtering, and drying the filter cake to obtain the fasudil hydrochloride refined product. According to the method, impurities in the fasudil hydrochloride can be effectively removed, the total impurity content is controlled to be 0.1% or below, the single impurity content is controlled to be 0.05% or below, the content is 99% or above, the pH value of the fasudil hydrochloride is effectively controlled to be 4.5-6.0, traditional column chromatography operation is avoided, and industrial production is facilitated.

The invention provides two preparation methods of 1, 7-dimethylxanthine, an intermediate thereof and a preparation method of the intermediate. The two preparation methods of 1, 7-dimethylxanthine, provided by the invention, have advantages of convenient operation, high safety, high atomic economy, fewer three wastes, cheapness, easy availability, low toxic, safe and stable raw and auxiliary materials, mild reaction conditions, fewer impurities and high yield; the preparation methods provided by the invention purify products by crystallization or beating, avoid column chromatography, and have advantages of simple and feasible operation, stable process, easy control, convenient reaction and post-treatment, and economical and convenient use for industrial production. The invention also provides a novel compound II and a preparation method of the compound II.

The invention relates to a synthesis process of a VEGFR (vascular endothelial growth factor receptor) inhibitor tevozanib. According to the invention, commercially available raw materials are subjected to a halogenation reaction, an esterification reaction and an addition reaction to synthesize a target product. Generally speaking, according to the synthetic route and the synthetic process, the synthetic steps are simplified, the reaction yield of each step is high, the treatment after the reaction is simple, pulping purification is mostly adopted for purification, the use of column chromatography is avoided, the operation process is simple and cheap, and the synthetic route and the synthetic process are favorably applied to industrial mass production.

The invention discloses a synthesis method of a dasatinib key intermediate. The synthesis method comprises the step of carrying out dehydration condensation reaction on a compound 2 and a compound 3 to generate a compound 4, i.e., the dasatinib key intermediate. By adopting the synthesis method of the dasatinib key intermediate, disclosed by the invention, the occurrence of side reaction is greatly reduced, the selectivity of the reaction is improved, and the final yield of dasatinib is improved; the synthesis method is suitable for industrial production. A formula is shown in the description.