48 results about "Aminopropionitrile" patented technology

The invention relates to a simple and quick method for synthesizing an improved vitamin B1 intermediate 2-methyl-4-amino-5-aminomethylpyrimidine. The method comprises the following steps: condensing 3-alkyl (aryl) formamido-propionitrile serving as a raw material with acetamidine in the catalytic action of lewis acid; cyclizing with trimethyl orthoformate, and hydrolyzing under an alkaline condition to prepare the vitamin B1 key intermediate 2-methyl-4-amino-5-aminomethylpyrimidine. The four reacting processes are performed in sequence by a one-pot reaction, and the product in each step does not need to be separated and purified. According to the method, highly carcinogenic o-chloroaniline or other small molecular aniline compounds are not used, residues of o-chloroaniline compounds in the vitamin B1 product can be eliminated. Furthermore, the preparation process is short and convenient in flow, small in wastewater amount and high in yield.

The invention relates to a simple and convenient preparation method of a key intermediate (2-methyl-4-amino-5-amino methyl pyrimidine) for the vitamin B1. According to the method, lewis acid is used for catalyzing addition condensation reaction of acetamidine and 3-formyl amino ethyl cyanide and then catalyzing reaction of the condensation product and triethyl orthoformate to introduce a formyl chiral auxiliary, an imdo group and the formyl chiral auxiliary are subjected to ring formation to form 2- methyl-4-formyl amino-5- amino methyl pyrimidine, and finally basic hydrolysis is performed, so that 2-methyl-4-amino-5-amino methyl pyrimidine is obtained. The reaction procedures are carried out sequentially by adopting the one-pot method, the products in each step require no separation and purification, and the operation is simple and convenient. According to the method, highly toxic o-chloroaniline and other phenylamine compounds are not used, so that residue of o-chloroaniline compounds in the vitamin B1 product can be completely avoided. Meanwhile, the production wastewater is less and the yield is high.

The invention discloses a process for preparing N,N-dimethyl-1,3-propane diamine through a continuous method and belongs to the field of organic chemical industry. The process comprises the following steps: by taking dimethylamine and acrylonitrile as raw materials, continuously preparing dimethylamino propionitrile by employing a fixed bed, wherein the molar ratio of dimethylamine to acrylonitrile is (10:1)-(1:1), the reaction temperature is 10-120 DEG C, the air speed is 0.1-10h<-1>, and the conversion rate of the acrylonitrile and the selectivity of the dimethylamino propionitrile are over 99 percent; and allowing the obtained dimethylamino propionitrile intermediate to directly enter a second fixed bed reactor for hydrogenating without any purification treatment, wherein the hydrogenation pressure is 3-10 MPa, a Raney-Ni catalyst is used, an alcoholic solution promoter with 0.1-10 percent of alkali is matched, the air speed is 0.1-4h<-1>, and the yield of N,N-dimethyl-1,3-propane diamine is not lower than 93 percent. The process for preparing N,N-dimethyl-1,3-propane diamine is simple, stable in quality, energy-saving and environment-friendly and is suitable for large-scale production.

The invention relates to the field of chemical synthesis and discloses a method for preparing D-calcium pantothenate. The method comprises the following steps of: reacting 3-aminopropionitrile with aqueous solution of sodium hydroxide or potassium hydroxide at the temperature of between 96 and 100 DEG C, adding hydrochloric acid to regulate the pH value, and concentrating and crystallizing; dissolving the prepared crystal by using methanol, and filtering to remove salt; and performing ion exchange with 732-type calcium ion exchange resin, carrying out acylation reaction between reaction liquid and D-pantolactone, crystallizing at the temperature of between 15 DEG C below zero and 10 DEG C below zero, and drying to prepare the D-calcium pantothenate, wherein the molar ratio of the 3-aminopropionitrile to the sodium hydroxide and the potassium hydroxide is 1:1.1-1.4, and the molar ratio of the 3-aminopropionitrile to the D-pantolactone 1:1-1.1. The method for preparing the D-calcium pantothenate has the advantages of not using calcium oxide or calcium hydroxide as a calcification agent, avoiding water generation in the reaction process so as to ensure the smooth acylation process, along with simple process, high yield, recycled 732-type calcium ion exchange resin, no generation of three wastes, and contribution to industrial production.

The invention belongs to the technical field of nitrile group hydrolysis and demethylation hydrolysis reaction which is one of the key steps for chemical synthesis of a methyldopa drug or a chiral drug of L-methyldopa [L-alpha-methyl-(3,4-dimethoxyphenyl)-alpha-aminopropionitrile, the same below], that is, a reaction for preparing alpha-methyl-(3,4-dimethoxyphenyl)-alpha-aminopropionitrile or L-alpha-methyl-(3,4-dimethoxyphenyl)-alpha-aminopropionitrile by nitrile group hydrolysis and demethylation hydrolysis. Under an acidic condition, the preparation of methyldopa by nitrile group hydrolysis and demethylation hydrolysis of alpha-methyl-(3,4-dimethoxyphenyl)-alpha-aminopropionitrile (or hydrochloride) requires a long period, a large material using amount, and heating hydrolysis of high-concentration acids (and the long-time heating of the high-concentration acids allows the acids to volatilize, so continuous acid addition is required during hydrolysis); however, the long-time high-concentration acid heating hydrolysis can cause unknown change of certain compound structures of alpha-methyl-(3,4-dimethoxyphenyl)-alpha-aminopropionitrile (or hydrochloride), and thus by-products are increased, and the purity and yield are decreased. Therefore, improvement of the hydrolysis technology is necessary.

The invention belongs to the technical field of beta-alanine, and relates to a continuous production process of beta-alanine. The method comprises the following steps: carrying out instantaneous hydrolysis reaction on the raw material beta-aminopropionitrile and liquid caustic soda through a micro-channel reactor under the conditions of high temperature and high pressure to obtain beta-sodium alanine-containing reaction feed liquid, then removing ammonia gas through a deamination system, exchanging sodium ions through an ion exchange system, and subjecting the exchanged beta-alanine aqueous solution to concentration crystallization to obtain beta-alanine, thus realizing continuous production from feeding to crystallization. According to the method, the reaction time is short, the side reaction occurrence probability is low, the product purity reaches 99.5% or above, and the yield reaches 95% or above; the whole system realizes automatic continuous production, is high in resource utilization rate, saves energy and reduces consumption.

The invention belongs to the technical field of one critical step in microwave nitrile hydrolysis and demethylation hydrolysis of chemical synthesis medicine methyldopa [alpha-methyl-(3,4-dyhydroxy phenyl)-alpha-aminopropionic acid, similarly hereinafter] or synthetic chiral medicine L-methyldopa [L-alpha-methyl-(3,4-dyhydroxy phenyl)-alpha-aminopropionic acid, similarly hereinafter], i.e. the chemical reaction for preparing methyldopa or L-methyldopa from alpha-methyl-(3,4-dimethoxy phenyl)-alpha-aminopropionitrile or L-alpha-methyl-(3,4-dimethoxy phenyl)-alpha-aminopropionitrile through microwave nitrile hydrolysis and demethylation hydrolysis. The microwave hydrolysis uses low-concentration hydrochloric acid or hydrobromic acid, so the energy sources and the economic cost are reduced, the acid wastewater discharge is reduced, by-products are reduced, and the purity and the yield of products are improved.

The invention provides a thoracoabdominal aortic aneurysm mouse model preparation method. The method includes: selecting a C57BL/6 mouse at the age of 9-11 weeks, and subcutaneously and continuously pumping BAPN (beta-aminopropionitrile) by 150mg/kg/day through an animal trace dosage osmotic pump for two weeks; subcutaneously and continuously pumping angiotensin II by 1000ng/kg/min through an animal trace dosage osmotic pump for six weeks to obtain a thoracoabdominal aortic aneurysm mouse model. By a beta-aminopropionitrile and angiotensin II combined method for inducing formation of thoracoabdominal aortic aneurysm of the C57BL/6 mouse, the established model better accords with a physiopathologic mechanism of thoracoabdominal aortic aneurysm formation, and further study on an aortic aneurysm pathological mechanism is benefited.

The invention discloses a process for continuously preparing N, N-dimethyl-1, 3-propane diamine by using micro-mixing and fixed bed reactors, and belongs to the technical field of organic chemical industry. A micro-mixing reactor and a fixed bed reactor are connected in series, and dimethylamine and acrylonitrile are used as raw materials to continuously prepare N, N-dimethyl-1, 3-propane diamine. By adopting the micro-mixing reactor, mass transfer and heat transfer of the reaction of dimethylamine and acrylonitrile are greatly improved, the reaction time of the first step is shortened to 0.3-4 min, and the probability of deterioration of the intermediate dimethylaminopropionitrile is reduced. Through the micro-mixing reactor, the gas-liquid raw materials in the second step are mixed more uniformly, the hydrogenation efficiency is improved, the yield of the prepared N, N-dimethyl-1, 3-propane diamine is greater than or equal to 98%, and the acrylonitrile conversion rate is greater than or equal to 99%. The process method can easily realize continuous production, low in cost, green, environment-friendly and suitable for industrial production.

The invention relates to a method for preparing beta-alanine through enzymatically catalyzing hydrolysis of high-concentration beta-aminopropionitrile. More specifically, the invention provides a hydrolyzing high-concentration beta-aminopropionitrile by utilizing nitrilase and genetically engineered bacteria thereof or combining together with aspartic acid lyase and genetically engineered bacteria thereof, and the beta-alanine is widely applied to synthesis of pantothenic acid, calcium pantothenate, carnosine, Pamidronate, balsalazine and other medical or feed and food additives. The method has the significant characteristics of being high in substrate concentration, mild in reaction conditions, pollution-free, simple in process route, and the like.

The invention discloses a process for continuously preparing N-hydroxyethyl-1, 3-propane diamine by using micro-mixing and a fixed bed reactor, and belongs to the technical field of organic chemical industry. The process comprises the following steps: taking ethanolamine and acrylonitrile as raw materials, firstly, continuously reacting through a first fixed bed reactor to generate an N-hydroxyethyl-3-aminopropionitrile intermediate, then, carrying out liquid-liquid mixing on the N-hydroxyethyl-3-aminopropionitrile intermediate and a cocatalyst in a first micro-mixing reactor, and then, carrying out gas-liquid mixing on the N-hydroxyethyl-3-aminopropionitrile intermediate and hydrogen in a second micro-mixing reactor together; finally, the intermediate reaction liquid continuously enters a second fixed bed hydrogenation reactor for catalytic hydrogenation, N-hydroxyethyl-1, 3-propane diamine is generated, and the yield is larger than or equal to 98%. The process is continuous in production, simple, less in three wastes, energy-saving, environment-friendly, low in cost and easy to industrialize.

The invention provides a method for preparing 3-aminopropionitrile from a waste liquid containing 3,3-iminodipropionitrile, wherein the method comprises the following steps: respectively introducing the waste liquid containing 3,3-iminodipropionitrile and an ammonia water solution into a micro-channel reactor to react, to obtain a reaction feed liquid; and carrying out deamination and distillation on the reaction feed liquid to obtain 3-aminopropionitrile. Firstly, the treatment method for preparing the 3-aminopropionitrile from the 3,3-iminodipropionitrile in the 3,3-iminodipropionitrile waste liquid can effectively realize reutilization of resources, and the yield of the 3-aminopropionitrile is relatively high; and secondly, the micro-channel reactor is adopted to strengthen mass and heat transfer in the reaction process, improve the reaction efficiency and realize continuous synthesis of the process, so that the high-temperature residence time can be shortened, the whole process is easy to control, the reutilization of beta-aminopropionitrile byproducts is improved favourably, and the consumption is reduced.

The invention relates to an environmental protection preparation method of 4-amino-2-chloro-3-nitropyridine. The method uses 3-amino propionitrile and trichloronitroethylene for 1,4-Addition and cyclization reaction to obtain 4-amino--2, 2, 3-trichloro-3-nitro-1, 2, 3, 6-tetrahydropyridine, and eliminates hydrogen chloride with an acid binding agent to prepare the 4-amino-2-chloro-3-nitropyridine.The method has the advantages of good reaction selectivity, good target product yield, high purity, short process flow, safe and simple operation, mild conditions, no waste acid and wastewater, environmental protection and low cost, and is carried out by a one-pot method.

The invention provides a preparation method and application of alpha-sodio formyl-beta-formylaminopropionitrile, and relates to the technical field of chemical synthesis. The preparation method of the alpha-sodio formyl-beta-formylaminopropionitrile comprises the following steps of: firstly, mixing beta-aminopropionitrile with methyl formate, and carrying out formylation reaction to obtain a pre-acylation solution; then sequentially adding sodium methoxide and isopropanol into the pre-acylation solution to be mixed, and conducting a synthetic reaction to obtain a solution containing alpha-sodium formyl-beta-formylaminopropionitrile; and finally, sequentially filtering and drying to obtain the alpha-sodio formyl-beta-formylaminopropionitrile. According to the preparation method, the sodio synthesis yield is effectively improved, and detection shows that the sodio synthesis yield can reach about 90% and is far higher than the existing sodio synthesis yield which is about 64%; and meanwhile, the preparation method also has the effects of reducing the consumption of methyl formate and reducing the generation of sodio mother liquor high-boiling residues.

The invention provides a preparation method and application of alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile, and relates to the technical field of chemical synthesis.The preparation method comprises the steps that an aqueous solution of alpha-sodium formyl-beta-formylaminopropionitrile and an acid solution of o-chloroaniline are subjected to a reaction, and alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile and o-chloroaniline are subjected to a reaction to obtain alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile; the alpha-(o-chloroaniline)-based methine-beta-formylamino propionitrile is obtained. The method solves the technical problems that solid alpha-sodium formyl-beta-formylaminopropionitrile is taken as a raw material in the traditional synthesis process, so that the operation environment is polluted by turnover throwing, the labor intensity is high, the operation period is long, the operation requirement is complex and the like; the technical effects of small operation environment pollution, simple operation, low labor intensity and short operation period are achieved.

The invention provides a preparation method of 6-chloro-4-trifluoromethyl-3-cyanopyridine, which comprises the following steps: by taking 2-chloro-3-trifluoromethyl acrylate (II) and 2-chloro-3-aminopropionitrile (III) as raw materials, carrying out addition reaction to obtain 2,4-dichloro-3-trifluoromethyl-4-cyano-5-amino valerate (IV), carrying out molecular lactamization reaction to obtain 3,5-dichloro-4-trifluoromethyl-5-cyano piperidine-2-one (V), then removing hydrogen chloride to obtain 6-hydroxy-4-trifluoromethyl-3-cyanopyridine (VI), and then carrying out chlorination reaction on VI and a chlorination reagent to obtain 6-chloro-4-trifluoromethyl-3-cyanopyridine (I). The raw materials used in the invention are cheap and easily available; the preparation and operation method is simple, small in wastewater amount, safe, environment-friendly and low in cost; the method has the advantages of high reaction selectivity, few byproducts and high target product yield and purity, and is suitable for green industrial production.

A use of aminopropionitrile in preparation of a medicine is provided. The medicine is used for treating late-stage hepatic fibrosis and cirrhosis. When compared with a contrast group free of aminopropionitrile, the medicine containing the aminopropionitrile can effectively reduce expression of fibrosis marker genes which are col lal, Acta2 and Desmin of mice with F3-stage hepatic fibrosis (based on METAVIR staging criteria), and can allow mouse liver tissue structures to be complete, collagenous fiber deposition to be reduced, collagenous fibers to be thinner, a collagen structure to be loose and dispersed, and activated astrocytes to be reduced, and therefore it is proved that the aminopropionitrile has obvious improving effects on hepatic fibrosis and cirrhosis.