70 results about "Sodium triacetoxyborohydride" patented technology

A novel process is provided for producing pramipexole base or its optical isomeric mixture as defined hereinabove i.e. (R,S)-2-amino-6-propyl-4,5,6,7-tetrahydrobenzothiazole avoiding the use of borane tetrahydrofuran complex and using a more convenient reducing agent like sodium triacetoxyborohydride instead. The provided process comprises reacting the starting material (S)-2,6-diamino-4,5,6,7-tetrahydrobenzothiazole or its optical isomeric mixture as defined hereinabove i.e. (R,S)-2,6-diamino-4,5,6,7-tetrahydrobenzothiazole with propionaldehyde in an organic solvent to obtain the respective enamine, which is subsequently reduced in situ, optionally without isolation, to obtain pramipexole or its optical isomeric mixture as defined hereinabove i.e. (R,S)-2-amino-6-propyl-4,5,6,7-tetrahydrobenzothiazole, and the acid addition salts thereof. The present invention also provides a process for purifying pramipexole dihydrochloride or the dihydrochloride salt of its optical isomeric mixture as defined hereinabove i.e. (R,S)-2-amino-6-propyl-4,5,6,7-tetrahydrobenzothiazole dihydrochloride by re-crystallization from a suitable solvent.

The invention discloses a ceramic metal material which is composed of following raw materials including 10-15 parts of ferric oxide, 10-15 parts of aluminium oxide, 5-12 parts of nano silicon dioxide, 100-150 parts of kaolin, 80-100 parts of quartz sand, 5-10 parts of zinc oxide, 50-60 parts of zircon, 5-10 parts of silicon nitride, 5-8 parts of aluminium nitride, 20-25 parts of hydroxyapatite, 10-15 parts of paraffin, 5-10 parts of lithium borohydride, 5-10 parts of potassium borohydride and 3-8 parts of sodium triacetoxyborohyride. In the ceramic metal material, the raw materials are reasonably blended. The ceramic metal material is excellent in performance, is good in stability, is high-temperature-resistant and corrosion-resistant, is good in water-proof performance, is high in strength and can be applied in various fields.

The invention relates to a method for synthesizing Varenicline intermediate 2, 3, 4, 5-tetralin-1, 5-methylene-hydrogen-benzoazepine. The method includes the following steps: under the action of catalyst, mixing amyl nitrite with o-aminobenzoic acid solution to generate diazonium salt, then mixing the diazonium salt with cyclopentadiene, and heating to react to generate compound 1; feeding ozone into the solution of compound 1, after complete conversion, adding reducing agent to generate compound 2, then dripping the compound 2 to the mixed solution of triacetoxy sodium borohydride and benzylamine to generate compound 3 by loop closing; and hydrogenating the compound 3 under the action of palladium and carbon for debenzylation and reduction to obtain M intermediate 2, 3, 4, 5-tetralin-1, 5-methylene-hydrogen-benzoazepine. The method has the advantages of greatly simplifying the method for preparing Varenicline intermediate, being simple in production process and safe in operation, well ensuring no harm to the environment and control on production cost, increasing yield and being capable of becoming a process in great industrial production.

The invention relates to a method for preparing amorolfine hydrochloride. The method comprises the following steps of: reacting 4-iodo-tert-amylbenzene with 2-methylallyl alcohol by taking N-methylpyrrolidone as a solvent in the presence of a palladium catalyst and alkali to obtain 3-tert-pentylphenyl-2-methyl propanal; performing reductive amination reaction of the obtained 3-tert-pentylphenyl-2-methyl propanal and cis-2,6-dimethylmorpholine by taking sodium triacetoxyborohydride as a reducing agent in the presence of glacial acetic acid to obtain amorolfine; and transforming the amorolfine into the amorolfine hydrochloride. The invention has the advantages that the process is reasonable, is beneficial to the environment, health, and safety (EHS), and is suitable for industrialized production, wastewater is easy to biodegrade, the reaction selectivity is high, the high-yield high-purity product is obtained, and the like.

The invention discloses an etimicin sulfate preparation method. The etimicin sulfate preparation method includes the steps of protecting amino groups at 3, 2', 6' and 3' of gentamicin C1a with Fmoc-Cl and performing purification and evaporation to dryness to obtain quadrifluorenyl methoxycarbonyl gentamicin C1a; adding N-ethyl of an acetaldehyde aqueous solution under acidic conditions and performing reduction with sodium triacetoxyborohydride; finally adding a piperidine/DMSO (dimethylsulfoxide) solution for deprotection; performing secondary purification on an reaction solution with weakly acidic cation adsorption resin after performing primary purification on the reaction solution with a macroporous adsorption resin column and adding sulfuric acid to a purified product to obtain etimicin sulfate through reaction. The etimicin sulfate preparation method is high in selectivity and less in side reaction in group protecting, mild in reaction conditions, simple in operation and easy to perform industrial production during the whole reaction process and high in purity and yield of the product. (An equation as shown in the description).

The invention discloses a new technology for preparing a key intermediate Hoffer's chlorosugar of telbivudine. The technology is characterized in that the technology comprises the following steps: 1, obtaining an epoxide by carrying out condensation, oxidation ring-opening, methylation, tosylation, reduction and epoxidation on vitamin C which is massively supplied in China and is treated as an initial raw material; 2, carrying out ring-opening cyaniding on the obtained epoxide; 3, carrying out sulfuric acid hydrolysis and lactonization on the generated cyan butanetriol derivative; and 4, carrying out hydroxy protection with p-toluoyl chloride, reducing with sodium triacetoxyborohydride to obtain a reduction product, and directly chloridizing the reduction product to obtain the target compound Hoffer's chlorosugar without separation, wherein the Hoffer's chlorosugar is 1-choro-3,5-bis-O-p-toluyl-2-deoxy-L-ribose. According to the technology, the total route yield is 42%, and the product purity is greater than 98%.

The present invention discloses a Teneligliptin synthesis method. The method comprises the following steps: (1) in the presence of an organic solvent and a catalyst of sodium triacetoxyborohydride, carrying out reduction on 1-[4-(3-methyl-1-phenyl-1H-pyrazol-5-yl)piperazine (in formula I) and 3-[(2S)-1-(1,1-dimethyl-acetyl carbonyl)-4-oxo-pyrrolidin-2-ylcarbonyl]thiazolidine (in formula II) into an intermediate (in formula III), wherein the solvent is a mixed solution of tetrahydrofuran and toluene; and (2) using sodium tablets to treat the mixed solution of tetrahydrofuran and toluene. According to the Teneligliptin prepared by the method disclosed by the present invention, the operation is simple, the yield is high, and the product purity is high; and the present method disclosed by the invention can remove basic impurities which require column chromatography to remove in the reaction, so that the process steps are simplified, the production cycle is shortened, and the total yield is relatively high; so that the synthesis method provided by the invention is more conducive to industrial production.

The invention discloses nanometer bismuth tungstate with a hollow square ball structure and a preparation method thereof. The preparation method is characterized in that a hollow square ball formed by stacked bismuth tungstate nanosheets is prepared by using bismuth nitrate pentahydrate as a bismuth source, sodium tungstate dihydrate as a tungsten source and an STAB (Sodium triacetoxyborohydride)-containing alcohol-water solution as a dispersing agent and utilizing ammonia water and sodium hydroxide under a hydrothermal condition, and the thicknesses of the nanosheets are about 30nm; and the inner diameter of the square ball is about 1.5 micrometers, and the outer diameter of the square ball is about 2 micrometers. The preparation method has the advantages of simplicity, easiness in operation, strong repeatability, environment protection, no toxicity and harmlessness in a preparation process, novel product morphology, high phase purity and the like and has a high application value in terms of pollution treatment, ray absorption and the like.

The invention discloses a novel synthesis process of prasugrel. The novel synthesis process comprises the steps: firstly, carrying out benzyl protection by taking 4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine, benzaldehyde and sodium triacetoxyborohydride as starting raw materials to generate 5-benzyl-4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine; then, brominating the 5-benzyl-4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine by using hydrobromic acid to obtain 2-bromo-5-benzyl-4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine; next, catalytically synthesizing 2-acetoxy-5-benzyl-4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine by taking palladium acetate as a catalyst and XPhos as a ligand; and finally, carrying out hydrodebenzylation, and coupling the product with alpha-bromo-o-fluorobenzyl cyclopropyl ketone to obtain a target molecule 2-acetoxy-5-(alpha-cyclopropylcarbonyl-2-fluorobenzyl)-4, 5, 6, 7-tetrahydrothieno[3, 2-c]pyridine hydrochloride, i.e., the prasugrel hydrochloride. The process is simple, convenient and novel in route, easy to obtain raw materials, mild in condition, convenient to operate, high in total yield up to 80-90% and suitable for large-scale production.

The invention discloses a ceramic metal material. The raw materials in parts by weight include: 5-10 parts of iron oxide, 10-15 parts of aluminum oxide, 6-10 parts of nano silicon dioxide, 80-120 parts of kaolin, and 80-120 parts of quartz sand 100 parts, 4-8 parts of zinc oxide, 30-50 parts of zircon, 4-8 parts of silicon nitride, 4-6 parts of aluminum nitride, 5-10 parts of molybdenum trioxide, 4-8 parts of magnesium, hydroxyapatite 15-25 parts of stone, 10-14 parts of paraffin, 10-15 parts of titanium, 10-14 parts of lithium borohydride, 4-8 parts of potassium borohydride, 3-5 parts of sodium triacetoxyborohydride, polystyrene particles 30‑40 servings. The composition of the present invention is reasonable, the ratio is coordinated, and the ceramic metal material produced has excellent performance, good stability, excellent high temperature resistance, corrosion resistance and waterproof performance, and can be used in various fields, and the present invention has good wettability, Reduce the fragility of the material and effectively enhance the strength of the material.

The invention provides a synthesis method of a gadoxetate disodium key precursor-(S-1-(4-ethyoxyl benzyl)-3-azapentane-1,5-diamine trihydrochloride. The synthesis method comprises the following steps: taking O-ethyl-N-Boc-L-tyrosine ethyl ester (a compound 1) as a material; reducing the material by red aluminum to obtain O)-ethyl-N-Boc-L-tyrosine aldehyde (a compound 2); then obtaining 1,5-Boc double-protection (S)-1-(4-ethyoxyl benzyl)-3-azapentane-1,5-diamine (a compound 3) by virtue of amination and reduction with N-Boc-1,2-ethanediamine under catalysis of sodium triacetoxyborohydride; finally, removing Boc protective groups through concentrated hydrochloric acid or a hydrogen chloride gas so as to obtain the (S)-1-(4-ethyoxyl benzyl)-3-azapentane-1,5-diamine trihydrochloride (a compound 4). According to the synthesis method disclosed by the invention, synthesis route steps are novel and concise, dear and dangerous special reagents are not needed, reaction is gentle, a product is easy to purify, after-treatment is convenient, and therefore, the synthetic method is suitable for industrial production.

The invention relates to a preparation method of a sitafloxacin hydrate five-membered ring side chain intermediate. The preparation method comprises following steps: keto carbonyl groups of a raw material 1 are reacted with sodium cyanoborohydride or sodium triacetoxyborohydride in the presence of ammonium acetate or ammonium chloride; reduction of amide carbonyl groups of an obtained production is realized with lithium aluminum hydride; free amino groups of a reduction product are reacted with di-tert-butyl dicarbonate ester in the presence of an alkali; phenethyl groups of an obtained compound are subjected to reductive destruction with formic acid or a formate in the presence of palladium-carbon so as to obtain the sitafloxacin hydrate intermediate (product 5). Reaction conditions of the preparation method are mild; equipment requirements are low; preparation process is safe; stereoselectivity is excellent; the raw material reagents are cheap and easily available; and production cost is low.

The invention belongs to the field of chemical conversion, and particularly discloses a method and a device for preparing selenocystine under mild conditions. The method specifically comprises the following steps: mixing selenium powder, a strong alkaline substance, water and sodium triacetoxyborohydride, adding a 3-chloro-L-alanine aqueous solution, and carrying out a stirring reaction; and afterthe reaction is finished, adding an acid, filtering, adding an alkali into the obtained filtrate to adjust the pH value, and carrying out standing filtering to obtain filter residues, ie., selenocystine. According to the invention, the method has the advantages of few side reactions, high raw material utilization rate, and almost no generation of hydrogen or other undesired reactions; and a sodium diselenide solution is prepared by using sodium triacetoxyborohydride as a reducing agent under a strong alkaline condition, so that the reaction is mild, safe and reliable, the operation is simpleand feasible, the reaction process is mild and controllable, and the method has good application prospect.

The invention discloses a preparation method of a B cell lymphoma factor-2 inhibitor ABT-199, and belongs to the field of pharmaceutical synthesis. The method comprises the following steps: substituting a starting material methyl 4-fluorosalicylate that is compound II with tert-butyl-1-piperazinecarboxylate that is compound III in the presence of a phase transfer catalyst, then de-protecting underthe acidic condition to obtain a compound IV, performing reductive amination on the compound IV and a synthesized key intermediate compound V in the presence of a catalyst (sodium triacetoxyborohydride) to obtain an intermediate VI, substituting the intermediate VI with a raw material VII that is 5-bromo-azaindole, then directly hydrolyzing and acidifying the obtained esterified product to obtainan intermediate VIII, and finally amidating the intermediate VIII and a raw material compound IX to obtain a target product compound I. The raw materials are easy to purchase or synthesize, the synthesis steps are short, the total yield is more than or equal to 40%, the use of expensive or difficult-to-purchase raw materials is avoided, and the method is suitable for industrial production.

The invention discloses an ursolic acid derivative, a preparation method thereof, and an application thereof in the preparation of a drug for treating methicillin-resistant Staphylococcus aureus (MRSA) infection. The preparation method comprises the following steps: oxidizing ursolic acid by a Sarrett reagent to obtain a 3-hydroxy oxidation product of ursolic acid, and carrying out reductive amination on the 3-hydroxy oxidation product of ursolic acid by isopropyl titanate and sodium triacetoxyborohydride in order to prepare the ursolic acid derivative. Anti-MRSA activity test proves that theMIC of the obtained ursolic acid derivative on MRSA test strains is 16-32 [mu]g/mL, the anti-MRSA activity of the ursolic acid derivative is 4-8 times higher than that of the ursolic acid, and the derivative can form a salt together with equimolar hydrochloric acid in order to significantly improve the water solubility. The ursolic acid derivative has a significant anti-MRSA activity and a good development prospect, and can be used to prepare the drug for treating the MRSA infection.

The invention discloses a preparation method and application of one group of pyrazolyl steroid derivative with antitumor activity, which belong to the technical field of medicine synthesis. The preparation method comprises the steps of generating phenylhydrazones 2 and 8 under the catalysis of isopregnenolone 1,5,16-diene progesterone and phenylhydrazine acetic acid; then carrying out ring closing reaction under the catalysis of phosphorus oxychloride to obtain compounds 3 and 9 with pyrazolyl heterocycle; then hydrolyzing to obtain compounds 4 and 10 without formyl groups; carrying out reduction with sodium borohydride to obtain 6; carrying out amination reduction reaction on the intermediate products 4 and 10 and amine under the catalysis of sodium triacetoxy borohydride to obtain 5a-e and 11a-e. The preparation method provided by the invention has the advantages of novel route, high yield and easiness for separation, and the route is an optimal route for preparing the compound.

The invention relates to a terminal modification method for improving redispersibility and suspension stability of cellulose nanocrystals. The method comprises the following steps: firstly mixing a cellulose nanocrystal suspension and a pH buffering solution such as a sodium carbonate solution, adding an amino-containing cyclic compound and a reducing agent such as sodium triacetoxyborohydride, and performing an aldehyde amine condensation reaction and a reduction reaction to bond reactive aldehyde groups at the terminal of the cellulose nanocrystals to amino and simultaneously reduce a carbon-nitrogen double bond into a more stable carbon-nitrogen single bond. According to the method provided by the invention, through the above modification, an original rod-like morphology and crystal structure of the cellulose nanocrystals and hydroxyl used as hydrogen bond driving force and a negative charge sulfonate group at the surface of the nanocrystals are retained, and the electrostatic repulsion effect of surface negative charges (the sulfonate group) and the steric hindrance effect of a terminal modified molecule (the cyclic compound) of the cellulose nanocrystals are fully utilized, sothat the redispersibility and stability in an aqueous suspension of the cellulose nanocrystals are efficiently improved.

The invention discloses a preparation method of 1-cyclohexylpiperazine. The method comprises the steps of carrying out reflux reaction on cyclohexyl halide, 1-Boc-piperazine and inorganic base in an organic solvent, filtering after the reaction is finished, and concentrating to obtain an intermediate 1; removing Boc from the intermediate 1 under an acidic condition, drying by distillation after the reaction is finished, pulping with isopropanol, and filtering to obtain solid 1-cyclohexyl piperazine hydrochloride; dissolving with water, adding an inorganic base to adjust the pH value to 12 to 14, extracting with an extraction solvent, drying the solvent by distillation to obtain a crude product of 1-cyclohexylpiperazine, and carrying out reduced pressure distillation on the crude product through an oil pump to obtain a pure product of 1-cyclohexylpiperazine. In the synthesis process of the intermediate 1, use of sodium triacetoxyborohydride and sodium hydroxide is avoided, the production cost is greatly saved, meanwhile, only filtering is needed for aftertreatment, the method is very simple, and time and labor are saved.

The invention provides a preparation method of brivaracetam, comprising the steps of (1) aminating, to be specific, dissolving compounds 2 and 3 in solvent 2, and stirring at controlled temperature of10-50 DEG C to allow reacting for 2-3 h, wherein the solvent 2 is one or more of methylbenzene, 1,2-dichloroethane, dichloromethane, trichloromethane and tetrahydrofuran; (2) reducing, to be specific, adding a reducing agent, and allowing reacting at controlled temperature of 10-50 DEG C for 1-4 h, wherein the reducing agent is one or more of sodium borohydride, potassium borohydride and sodium triacetoxyborohydride; (3) performing lactamization, to be specific, allowing reacting at controlled temperature of 20-100 DEG C for 2-5 h, wherein the steps (1) to (3) are performed in inert gas environment. The intermediate compounds of brivaracetam used herein are low in price, and the preparation method has mild reaction conditions and is suitable for industrial large-scale production.

A metal ceramic material is prepared from the following raw materials in parts by weight: 6-13 parts of iron oxide, 6-14 parts of hydroxyapatite, 4-10 parts of lithium borohydride, 3-10 parts of sodium triacetoxyborohydride, 1-4 parts of Fe, 2-5 parts of Mn, 3-10 parts of rutile type titanium dioxide, 3-8 parts of quartz, 2.5-9 parts of a razor clam king shell powder, 1-3 parts of boron glass, 4.2-6 parts of calcium hydrogen phosphate, 3-6 parts of agate, 3.5-10 parts of borax decahydrate, 5-8 parts of nano ferrum dioxide, 1-4 parts of magnesium oxide, and 6-13 parts of barium hydroxide. The metal ceramic material has the beneficial effects that the metal ceramic material has the characteristics of small density, high hardness and quite good high-temperature stability, and improves the service life of ceramics.

The invention provides a preparation method for N-(2- indanyl) glycine alkyl ester. An N-(2- indanyl) glycine alkyl ester crude product is obtained through the reaction of glycine alkyl ester and 2-indenone, and the reducer used in the reaction of the glycine alkyl ester and 2-indenone is triacetyl oxygroup sodium boro-hydride; and the molar ratio of 2-indenone and triacetyl oxygroup sodium boro-hydride is 1 to 0.79 to 1.59. By adopting the method, NaBH (OAc) 3 is used for preventing the use of NaBH3CN, the production of toxic substance is avoided, and the yield of the prepared N-(2- indanyl) glycine alkyl ester can reach 77.2 percent.