219results about How to "Short synthetic steps" patented technology

The invention relates to a method for preparing praziquantel, which is characterized by comprising the steps: (1) isoquinolin, sodium cyanide or potassuim cyanide and triethylamine or pyridine are added into a reactor to react, and yellow solid which is a first step product is obtained; (2) the first step product is added into a high-pressure hydrogenation kettle and filled with hydrogen to react under the action of catalyst, so that a second step product is obtained; (3) after being stirred and dissolved, the second step product and ethyl acetate is added with anhydrous potassium carbonate or anhydrous sodium carbonate, and then is stirred at the room temperature and dripped with chloracetyl chloride to be stirred at the room temperature to react, so that the solid obtained in the reaction is crude product of the praziquantel, and fine product is obtained by recrystallization of absolute methanol. Compared with the prior art, the method has the advantages of shortening the reaction process, reducing the energy consumption, improving the overall yield, etc.

The invention discloses a preparation method of apremilast (+)-2-[1-(3-ethoxy-4-methoxyphenyl)-2-mesylethyl]-4-acetamidoisoindolinyl-1,3-dione. The method comprises the following steps: (1) converting a compound 1-(3-ethoxy-4-methoxyphenyl)-2-(methanesulfonyl)ethylamine racemate disclosed as Formula (II) into a salification substance disclosed as Formula (III) by using a resolving agent; and (2) connecting the compound disclosed as Formula (III) with 3-acetamidophthalic anhydride to obtain the compound disclosed as Formula (I). The method can be utilized to obtain the stable apremilast acceptable finished product, has the advantages of mild technological conditions, simple after-treatment, high purity and low reaction cost, and can easily implement industrial production.

The invention provides a method for synthesizing febuxostat. The method comprises the following steps of: (a) performing aromatic ring substitution reaction on a compound of a formula I to obtain a compound of a formula II; (b) performing halogen-metal exchange reaction on the compound of the formula II to obtain a compound of a formula III; (c) performing coupling reaction on the compound of the formula III and the compound of a formula VI under the action of a metal catalyst to obtain a compound of a formula IV; and (d) performing hydrolysis reaction on the compound of the formula IV to obtain the compound of a formula V, namely febuxostat, wherein X is I or Br; M is selected from boric acid ester or SnBu3; and R is H or an alkyl group. In the method, a convergent synthesis strategy is adopted, and a carbon-carbon bond is formed by applying metal catalyzed aromatic ring coupling reaction in a key step, so that a system in which a benzene ring is coupled with a thiazole ring is established. The method has the advantages of simple and short steps, high yield and low environmental pollution and can be suitable for industrial production.

The invention discloses a synthetic method of sitagliptin and a salt thereof. The synthetic method comprises the steps: carrying out an esterification reaction, a reduction reaction, an oxidizing reaction and a witting reaction on 2,4,5-trifluorophenylacetic acid as a starting raw material to obtain 4-(2,4,5-trifluorophenyl)-2-ethyl crotonate; then carrying out a hydroamination reaction on 4-(2,4,5-trifluorophenyl)-2-ethyl crotonate and chiral amine in the presence of butyl lithium or hexamethyldisilazane sodium to form a chiral hydroamination product; carrying out an esterolysis reaction, a condensation reaction and a hydrogenation reaction to obtain sitagliptin. The raw materials used in the synthetic method of sitagliptin are low in price and easy to obtain; the synthetic method of sitagliptin is less in step, easy to operate and capable of effectively reducing cost. By the use of the method, high-purity sitagliptin can be obtained, a sitgliptin phosphate obtained through salifying has an HPLC (High Performance Liquid Chromatography) and an ee (enantiomeric excess) value of more than 99% and can be applied to the field of medicine.

The invention provides a novel Michler ketone-cyan organic dye and a synthetic method thereof. The dye derives from Michler ketone, and has the structural formulae which represent Michler ketone-cyan organic dye compounds 1, 2, 3, 4 and 5, respectively. Each molecule of the dye comprises two nitrogen containing groups, namely, the structural feature of double electron-donating groups. Accordingly, the molecules can be oxidized and deacidized easily, and have better capability of donating electrons and the capability of trapping electrons from electrolyte more quickly. The dye extends the design thought of organic photosensitizers, and enriches the research content of dye sensitization solar batteries, thereby having very important significances for improving the photoelectric transformation efficiency of organic solar batteries and reducing the cost of batteries both in theory and practice. The synthetic step is short, the process is simple; the cost is low and the yield is high.

The invention discloses a synthesis method for (2'R)-2'-deoxy-2'-fluorine-2'-methyl uridine, which comprises the following steps: in the presence of an organic solvent and Lewis acid, enabling (R)-3-F-3-methyl furan to react with 2,4-(di-hydroxyl protection) pyrimidine at 25-100DEG C; after the reaction is finished, processing a reaction product to obtain a compound (IV); and performing dehydroxylation protection to obtain the (2'R)-2'-deoxy-2'-fluorine-2'-methyl uridine (V). When adopted to synthesize the (2'R)-2'-deoxy-2'-fluorine-2'-methyl uridine, the method has short synthesis steps, is simple and convenient to operate and has important application values.

The invention discloses a preparation method of alpha-crystal form imatinib mesylate. The preparation method comprises the following steps that 1, 4-[(4-methyl piperazine-1-yl)methyl]benzoic acid dihydrochloride shown in the formula II is converted into an acyl chloride shown in the formula III by an acylating chlorination reagent; 2, the acyl chloride shown in the formula III and N-(5-amino-2-methylphenyl)-4-(3-pyridyl)-2-aminopyrimidin undergo a condensation reaction in the presence of an alkali to produce a compound shown in the formula IV; and 3, the compound shown in the formula IV and methylsulfonic acid undergo a salt forming reaction in the presence of an organic solvent to produce a compound shown in the formula I. The preparation method can realize preparation of stable alpha-crystal form imatinib mesylate and allows mild process conditions. The stable alpha-crystal form imatinib mesylate can be after-treated simply and has high purity. The preparation method has a low reaction cost and is suitable for industrial production.

The invention relates to a preparation method of (S)-equol, which aims to solve the problem of complex operation in the existing preparation method of (S)-equol. The preparation method comprises the following steps: by using daidzein as the main material, carrying out hydroxy protection, catalytic hydrogenation, dehydration and chiral catalytic reduction to prepare the (S)-equol. The invention has the advantages of cheap and accessible raw materials and low cost, is simple to operate, and is suitable for industrial scale-up production; and the yield is 60-70%. The invention is applicable to the field of synthesis of medicine compounds.

The present invention relates to a 1, 5, 9-trisubstituted coronene compound and a synthesis method thereof. The structural formula of the compound is shown in img file = 'dest _ path _ image 001. TIF 'wi = '109 'he = '108', wherein R represents H, C1-C18 alkyl, phenyl, 4-methylphenyl, 4-methoxy phenyl, benzyl, cyclohexyl, 4-trifluoromethylphenyl, thiophene, furan and the like. According to the technical scheme of the invention, the easily prepared 1, 5, 9-triamido triphenylene is subjected to diazotization and halogenation reaction to obtain the tri-halogenated triphenylene. After that, the tri-halogenated triphenylene is subjected to Sonogashira reaction with various alkynes to generate atriyne-triphenylene compounds. Finally, through the metal-catalyzed reaction and the cyclization reaction under the effect of an organic base, various 1, 5, 9-trisubstituted coronene compounds, novel in structure, can be obtained. According to the technical scheme of the invention, raw materials are easy for mass preparation. Meanwhile, the synthesis step is relatively short and the operation is convenient. The obtained trisubstituted coronene compound is good in thermal stability and chemical stability, and the trisubstituted coronene emits the relatively strong fluorescence within the range of 420-550 nm according to the fluorescence emission spectrum of the trisubstituted coronene compound. Therefore, the trisubstituted coronene is an excellent fluorescent material for preparing UV ultraviolet charge-coupled devices (UV-CCD) and organic light-emitting diodes (OLEDs), and has a wide application prospect in the field of electronic materials.

The invention relates to a method for preparing L-glufosinate-ammonium. According to the method, cheap and easily available L-homoserine is used as an initial raw material, L-glufosinate-ammonium witha high ee value is prepared through a three-step reaction, chiral catalysis is not needed, the cost is low, and the method has a potential industrial application value.

The present invention relates to a method for rapidly preparing a remdesivir intermediate represented by a following formula (I) without complex purification and separation, wherein X represents a halogen element. The method is simple, high in yield and single in product, and can be obtained through simple filtration and separation; complicated separation operation such as column chromatography isnot needed; the remdesivir intermediate represented by the formula (I) can be rapidly, efficiently, and massively prepared; and sufficient intermediates are provided for large-scale preparation of remdesivir drugs that may be used to treat new corona viruses.

The invention belongs to the technical field of medicines, and relates to a method for synthesizing lorlatinib (PF-06463922), which is finally synthesized from 5-fluoro-3-methyl isobenzofuran-1(3H)-ketone and 1-methyl-3-((methylamino)methyl)-1H-pyrazol-5-nitrile through the reacting steps including aminolysis, substitution, coupling, chiral resolution and the like, or from (S)-5-fluoro-3-methyl isobenzofuran-1(3H)-ketone and 1-methyl-3-((methylamino)methyl)-1H-pyrazol-5-nitrile through the reacting steps including aminolysis, substitution, coupling and the like. According to the method, a novel method is provided to synthesis of an anti-tumor medicine lorlatinib (PF-06463922).

The invention belongs to the field of medicine synthesis and particularly provides a preparation method for Sitagliptin. According to the method, a cheap metal ruthenium complex and cheap R-BINAP serve as ligands, and the asymmetric hydrogenation reduction of an enamine intermediate is catalyzed, so that R-configuration Sitagliptin can be obtained in a high-selectivity manner; and the reaction time is short, and both the yield of reduction and the ee value of the product are relatively high, so that the method is applicable to industrialized amplified production.

The invention discloses a method for preparing a mitochondria targeted spinning scavenger MitoPBNs (spinning probe). The structural formula of the MitoPBN is shown in a formula (I). A synthesis flow is shown in the formula (II), and comprises the following steps of: performing elimination reaction on 4-hydroxybenzaldehyde and dibromo-straight-chain paraffin under alkali condition to prepare a compound 3; reacting the compound 3 with triphenylphosphine to prepare the compound 4; in ethanol, mixing the compound 4, 2-nitro-2-methylpropane, a 4A molecular sieve and zinc powder in a solvent, adding dropwise a glacial acetic acid, stirring and reacting the mixed solution at room temperature, placing the mixed solution in a refrigerator for refrigeration, and performing separation and purification to prepare the spinning probe MitoPBN; and performing liposome packing treatment. The method has the characteristics of relatively fewer synthesis steps, low raw material cost, readily available raw materials and relatively higher product purity. The probe for scavenging free radical signals can enter cell mitochondria.

The invention relates to a method for synthesizing a repaglinide key intermediate, namely 4-ethoxycarbonyl-3-ethyoxy phenylacetic acid. The method comprises the following steps: by taking 3-ethyoxy-4-ethoxycarbonyl-benzyl cyanide as an initial raw material, performing hydrolysis, esterification, selective hydrolysis and the like, thereby obtaining the important intermediate 4-ethoxycarbonyl-3-ethyoxy phenylacetic acid of repaglinide. According to the key intermediate, the impurities of the product is less, the purity of the product is high and can reach over 99.7%, so that the quality of the subsequently synthesized repaglinide product is improved, the 100 percent first-pass yield of the subsequently synthesized repaglinide product can be basically reached, a refining step is avoided, and the synthetic yield is effectively improved. The process is easy and convenient to operate, the yield is high, the molar yield is 69.1 percent, the production cost is low, and the method is suitable for industrial production.

The invention discloses a topiroxostat preparation method. According to the method, 2-chloroisonicotinic acid which is cheap and easy to obtain serves as an initial material, potassium ferrocyanide serves as a green cyanogens source, AgI-KI-PEG generates 2-cyanoisonicotinate through cyanation of a mixed catalysis system and then directly acts with hydrazine hydrate to obtain 2-cyanoisonicotinate hydrazide under the action of an amide condensing agent phenyl dichlorophosphate (PDCP), and the product and 4-cyanopyridine are condensed to obtain topiroxostat. Through technological improvement of the reaction, reaction steps are shortened, the reaction yield is obviously increased by 90% or above, and the technological cost is obviously reduced. Meanwhile, a 2-chloroisonicotinic acid raw material which is cheaper and easy to obtain is used, use of corrosive thionyl chloride and other chlorinating agents is avoided, and the technology is suitable for industrial production. The method is short in synthesis step, easy to operate, mild in reaction condition, economical, environmentally friendly and suitable for industrial production, and the yield is obviously increased.

The invention discloses a synthesis method of 2-(4-alkylphenyl) propionic acid, which comprises the following steps of: carrying out Friedel-Crafts reaction between ethyl 2-chloro-propionate and alkyl benzene with anhydrous aluminum chloride as a catalyst to obtain an intermediate product ethyl 2-(4-alkylphenyl) propionate; and hydrolyzing the intermediate product to obtain 2-(4-alkylphenyl) propionic acid. The invention has the advantages of short synthesis step, low reaction condition, and no need for high temperature or high pressure; the atom utilization rate is high, and the invention can lower energy consumption and reduce waste discharge, meeting the requirement of green chemistry on chemical production; and inexpensive common anhydrous aluminum chloride is used as a catalyst, thus lowering the production cost; moreover, the anhydrous aluminum chloride is especially suitable for producing brufen.

The invention relates to a high-efficiency high-stereoselectivity semisynthesis method of harringtonine and allied alkaloids, which uses optical pure cephalotaxin serving as a raw material to perform reactive synthesis with substituted silicon ketene in Lewis acid catalysis. The structural general formula of the compound is shown as (A), wherein the meaning of each group is shown as the specification. The method has the advantages of high chemical yield and diastereoselectivity of key reactions, convenient operation, short synthesis steps and the like. The method is a universal method for synthesizing the optical pure compound with the structural general formula shown as (A), and is suitable for massive preparation. The compound is widely applied to anti-tumor (malignant and non-malignant tumors), anti-parasitic, antifungal and antimicrobial chemotherapy medicaments.

The invention provides a preparation method of Mn<4+>-activated fluoride fluorescent powder. The preparation method provided by the invention does not need to form a saturated solution of A2MF6, so that the requirement of the use amount of raw materials is greatly reduced; in the preparation process, the target product can be synthesized at room temperature and is convenient to synthesize; a precipitating agent is added, so that the preparation is more convenient, the operation is simpler, the synthetic steps are simplified, and the prepared fluorescent powder has better optical properties; the fluoride fluorescent powder can be well excited by ultraviolet light to blue light, especially the blue light, and has strong red light emission, wherein the red light emission peak is in the wavelength range from 600 to 650 nm; the method has the advantages of a simple preparation process and short consumed time; and the prepared material has a high luminescence quantum yield and is suitable for industrial large-scale preparation.

The invention discloses a method for synthesizing deuterated tazobactam. The method comprises the following steps: adding 2beta-azomethylpenicillanic acid-1beta-oxide, propiolic acid, a catalyst containing copper or cuprous ion and sodium ascorbate in a deuterated solvent in turn, stirring at 25-200 DEG C for reaction for 1 to 48 hours, and after the reaction, performing extraction, filtering and column chromatography to obtain the deuterated tazobactam. Through the method, according to the method for synthesizing the deuterated tazobactam, the deuterated tazobactam is a novel beta-lactamase inhibitor of the penicillanic sulfone type and can be used for treating various bacterial infections; the method has the characteristics of mild reaction condition, short synthesis procedure, simple process and high yield, the safety during the reaction is effectively improved by using propiolic acid as the raw material, and the carbon-deuterium chain in the obtained deuterated tazobactam molecule is so stable that the medicine decomposition process can be effectively retained, therefore, the deuterated tazobactam has a longer action time in the body and is better than the normal tazobactam.