64 results about "Tropine" patented technology

The invention relates to the application of microwave and ultrasonic technologies in synthesizing tiotropium bromide anhydride, in particular to a method for preparing the refined product of a finished product, namely, tiotropium bromide anhydride through crystallization and recrystallization processes by using a crude product of tiotropium bromide prepared through bromization reaction after hydrolytic reaction of scopolamine hydrobromide under microwave function, substitution and coupling reaction of bromothiophene, magnesium, and oxalic acid dimethyl ester under the microwave function, and condensation reaction of scopine and thiophen methyl glycollate under the microwave function. Using the invention to prepare tiotropium bromide anhydride, not only the reaction time is short, the side reaction is less, and the yield rate is high in the room temperature condition, but also the product quality is stable, controllable, safe and effective.

The invention discloses a method for synthesizing an SAPO-35 molecular sieve by a two-mode agent, which is characterized in that the method comprises the steps of mixing aluminum source, phosphorus source, silicon source and an organic template to glue at the temperature of room temperature to 100 DEG C and preparing into the reaction mixture with the molar ratio components of a1R1+a2R2: Al2O3: bP2O5: cSiO2: dH2O, wherein R1 and R2 are the organic templates, the value of a1 is 0.5-1.8, the value of a2 is 0.1-1.0, the value of b is 0.5-1.5, the value of c is 0.05-2.5, and the value of d is 10-150; the reaction mixture undergoes hydrothermal crystallization for 0.5-500 hours at the temperature of 150-250 DEG C and the crystallization product is recovered. The R1 is hexamethylene imine, and the R2 is any of cyclohexane, piperidine, tropine, diethylamine and triethylamine. The method provided by the invention can synthesize the high-crystallinity SAPO-35 molecular sieve in a relatively wide silica content range. The SAPO-35 molecular sieve synthesized by the method of the invention is applicable to the hydrocarbon conversion technology. Applied to the olefin preparation reaction by methanol dehydration, the molecular sieve has very low alkane selectivity and high product yield of ethylene and propylene.

The invention discloses an analysis method for determining the hydroxamamide tropine raw drug content through a non-aqueous titration method and relates to the hydroxamamide tropine raw drug quality control technology field. The method for determining the content of hydroxamamide tropine is provided, the process of which is as follows: glacial acetic acid-acetic oxide is used as a solvent for the quantitative dissolution of the hydroxamamide tropine. Then, perrchloric acid titrating solution is sued as titrant, and a potentiometric titration method is adopted for the titration. The method has the advantages of small sample amount, simple operation, good precision, and the like, and can be applied to the routine analysis and the quality control of hydroxamamide tropine raw drugs.

The invention relates to a detection method for alpha-tropine as impurity in hydrochloric acid tropisetron, which is characterized by adopting the gas chromatography for detection, and particularly includes the following steps: (1) preparing sample hydrochloric acid tropisetron solution with concentration of 10mg/m1 to 30mg/ml; (2) preparing reference sample alpha-tropine solution with the concentration of 0.02mg/m1 to 0.06mg/m1; (3) performing headspace sample injection and chromatogram acquisition; and (4) calculating the result through the appearance method based on the peak area. The invention has the characteristics that the detection method is convenient, quantitative and sensitive, and can be widely applied to the control and improvement of the medicine quality.

The invention discloses an improvement method of a nortropine synthesizing process. In the method, tropine and ethyl chloroformate are adopted as raw materials to synthesize nortropine. By adjusting the experimental operating steps, the method achieves the effects of moderate reaction condition, safe, simple as well as convenient operation, good product quality, and low cost.

The invention relates to a novel method for producing and preparing nor-tropine. The method comprises the following steps: taking N-alkoxycarbonyl nor-tropine as a raw material, adopting a small amount of potassium hydroxide (2-10 equivalent weights); rapidly hydrolyzing at the temperature of 100-160 DEG C and at high pressure of 1-10 atmospheric pressure and cooling to -5 to 10 DEG C after finishing reaction; filtering the collected and precipitated product; and carrying out recrystallization by ethyl acetate to obtain the product with purity being more than 99%. The products are all in extravert-type structure by GC detection. The method has the following advantages: 1. reducing the dosage of the potassium hydroxide to 10-25% of original dosage, thus saving the cost; 2. leaving out the cumbersome operation of chloroform and extraction, saving solvent, saving a large number of manpower and reducing pollution; 3. the actual pressure is about 5kg which is safe relatively when a high pressure autoclave is operated, thus eliminating explosion risk generated by the reaction of chloroform and potassium hydroxide; and 4. the color and luster and purity of the product is higher.

The invention relates to a content analysis method for sulfhydryl-amine tropine. It uses high efficiency liquid phase chromatogram-vaporizing light scattering detector to test sulfhydryl-amine tropine. The devices that are used for chromatographic analyzing are WATERS 600 high efficiency liquid phase chromatograph, WATERS 2420 vaporizing light scattering detector, and the chromatographic column of Hypersil C8 column, 5um, 4.6*250mm. The results shows that it has good separation of the main constituents peak and the impurity peak, the linear range is 12.5-50ug/mL, and the minimum detecting quality is 3.0ng (S/N>=3), and that has about 3.6% error compared to relative standard error. The invention could test content and impurity of sulfhydryl-amine tropine, and it is simple and convenient.

Nimbin is extracted from nim kernel and has both pesticidal and bacteriostasis functions. Tropine is a kind of alkaloid extracted from solanaceae plant, such as henbane seed, belladonna and datura flower, and has powerful pesticidal function. Recompounding nimbin and tropine can obtain synergistic pesticidal effect. The nimbin-tropine emulsion of the present invention is recompounded with nimbin and tropine as main components and through adding proper amount of assistant. The pesticide has high efficiency, low toxicity, no pollution, safety to human body and farm animal and less resistance and may be used in preventing and treating various pests with resistance to other pesticides.

The invention provides a synthesis method of atropine and atropine sulfate, which comprises the following steps: carrying out acetylation reaction on tropine acid to form acetyl tropine acid, reactingthe acetyl tropine acid with a chlorination reagent to form acyl chloride, reacting the acyl chloride with tropine alcohol, removing acetyl to obtain atropine, and salifying atropine and sulfuric acid to obtain atropine sulfate. The whole synthesis process can be completed by adopting a one-pot reaction, additional steps for completing the process by isolating intermediates are avoided, the reaction conditions are mild, the steps are simple, the yield is high, the purity is high, and the method is suitable for large-scale industrial production.

The invention discloses a method for preparing 2-hydroxy-2,2-diphenylacetic acid-3alpha-(8-aza-bicyclo(3,2,1))-3-trioctyl. The method comprises the following steps of: by taking dibenzoyl as a raw material, carrying out rearrangement on the raw material so as to obtain dihydroxy-phenylacetic acid; reacting dihydroxy-phenylacetic acid with dimethyl carbonate under the DBU catalysis and microwave actions so as to obtain methyl benzilate; reacting the methyl benzilate with tropine so as to obtain tropine benzilate; and carrying out N formylation and alcoholysis on the obtained tropine benzilate so as to obtain nor-tropine benzilate. Compared with the prior art, the total reaction time of the method disclosed by the invention is greatly reduced, the total yield is increased greatly, and the reaction condition is more simple, and therefore, the method is suitable for industrial production.

The invention discloses a compound bonding agent for a baking-free magnesium vibration material. The compound bonding agent is composed of the following components by mass percent: 86.35 wt% of anhydrous dextrose, 4.55 wt% of borax, 4.55 wt% of tropine and 4.55 wt% of industrial salt. The bonding agent is the non-toxic, tasteless and nuisanceless white crystalline particles or powder, has strong basicity, is easily dissolved in water, and is insoluble in alcohol and acid, the aqueous solution of the bonding agent is alkaline, and the bonding agent belongs to inorganic salt products. No elements polluting molten steel exist, no toxic or harmful gas is produced during heating the bonding agent, occupational safety and health of workers cannot be influenced, and no pollution to the environment is caused.

The invention discloses a method for inspecting alpha-tropine related substance and isomer inspecting method by a thin-layer chromatography. By means of preparing a related substance and isomer reference substance solution, a sample loading amount is controlled; after a developer is spread, a color developing agent is sprayed; thus, tropine related substance and isomer can be controlled under 0.5%. The method has the advantages of simpleness in operation, convenience and quickness; dedicated inspecting instruments are avoided; an economical, practical and effective method is provided for quick detection on tropine.

The invention discloses a preparation method of tropisetron hydrochloride. The Preparation method of the tropisetron hydrochloride is characterized by comprising the following preparation steps: (A) performing substation reaction on 3-indolecarboxylic acid (I) serving as a starting material and thionyl chloride by adding a reaction solvent to prepare 3-indoleformyl chloride (II), and directly performing condensation reaction on the 3-indoleformyl chloride (II) and alpha-tropine (III) under the existence of an acid-binding agent triethylamine to produce tropisetron (IV); and (B) performing acid and alkali salt-forming reaction on the tropisetron (IV) and hydrochloric acid in ethanol to produce the tropisetron hydrochloride (V). Raw materials used in the process reactions are the conventional reagents, are easily available on the market and are low in cost; the conditions are simple and not harsh, the conventional equipment can meet production requirements and are easy to control, and industrialized production can be realized; and dichloromethane and tetrahydrofuran have low boiling point and are easily evaporated to dryness, so energy conservation and safety are achieved.

The invention relates to a 3 alpha-high tropine aliphatic amine salt, crystal formation and preparation method, which is to resolve problems of poor stability for preparing midbody of Granisetron, inconvenience for storage and transportation and low purity of final products. The 3 alpha-high tropine aliphatic amine is dissolved in one or more organic solvents and 1-10 equivalent hydrochloric acid, sulphuric acid or phosphoric acid are added in for crystallization and filtration after mixing to cool. 1 to 20-fold water and 10 to 100-fold alcohols solvent are used for recrystallization for cooling, crystallization, filtration and vacuum drying for 12 hours.

The invention discloses a synthesis method of a homatropine hydrobromide shown in a formula (V), comprising the following steps of: tropine shown in a formula (I) and a compound (III) obtained by esterification of O-formyl almond acyl chloride shown in a formula (II); acidic hydrolysis is carried out to the compound (III) to obtain a compound (IV); and the compound (IV) is salified by the hydrobromide to obtain a compound (V). The synthesis method has the beneficial effects of: avoiding the use of benzene as a toxic solvent, having mild reaction condition, simple operation, short production period, high reaction yield and low production cost, being applicable to industrial production and having larger implement value and social and economical benefits.

The invention belongs to the field of chemical synthesis, and particularly relates to a preparation method of atropine sulfate. The preparation method comprises the following steps: firstly preparing tropine ester, then preparing atropine, salifying to prepare atropine sulfate, and finally refining to obtain the product. In the preparation process of the tropine ester, the reaction temperature is strictly controlled to be 105-111 DEG C, and the crystallization temperature is controlled to be 0-5 DEG C, so that the yield of the tropine ester is improved. In the process of preparing atropine through reduction reaction, palladium-carbon is adopted as a catalyst, and the reaction temperature is strictly controlled to be 10-15 DEG C, so that the product quality is effectively improved. Sulfuric acid is diluted by preparing a sulfuric acid ethanol solution, and the dripping speed of the sulfuric acid ethanol solution is controlled, so that the stable quality of atropine sulfate is ensured.