25 results about "Alkyl nitrites" patented technology

The invention discloses a method for synthesizing alkyl carbonate through gas-phase carbonylation. Comprising a dechlorination method and a chlorine circulation process in the process of preparing alkyl carbonate through a gas-phase oxidative carbonylation reaction of carbon monoxide and alkyl nitrite. The content of water and alkyl alcohol in circulating gas is controlled through solvent absorption, alkyl chloride is synthesized with a chlorine supplementing agent HCl and alkyl chloroformate under the action of a dechlorinating agent, and the alkyl chloride is separated from a product through gas-liquid separation. When alkyl carbonate is produced by adopting the dechlorination method and the dechlorination process, the problem of equipment corrosion caused by chlorides can be avoided, the dechlorination process is a low-cost and environment-friendly chlorine circulation process, and stable operation of an industrial device is realized.

The application provides a synthesis method of p-benzoquinone dioxime. The synthesis method comprises the following steps: (1) adding solid acid into an ethanol solution of phenol to obtain a mixed solution A, then vacuumizing and filling with inert gas; dissolving nitrite into ethanol, uniformly mixing to obtain an ethanol solution of nitrite, then vacuumizing and filling with inert gas; in an inert gas atmosphere, adding the ethanol solution of nitrite into the mixed solution A dropwise to perform nitrosation reaction, to obtain a reaction liquid B; in the inert gas atmosphere, adding an ethanol solution of hydroxylamine into the obtained reaction liquid B to perform oximation reaction; after the reaction is completed, filtering the obtained reaction liquid C, performing reduced pressure distillation on the obtained filtrate, and performing washing, filtering and drying on the obtained residual liquid of the reduced pressure distillation, to obtain p-benzoquinone dioxime. The method provided by the application reduces the occurrence of side reactions, improves the conversion rate of the reaction, and improves the yield and purity of p-benzoquinone dioxime.

The invention belongs to the technical field of organic synthesis, and particularly relates to a synthesis method of an isoxazoline compound. The preparation method comprises the following steps: dissolving a compound 1 and ethyl acrylate in dichloroethane, then adding tert-butyl nitrite, alkali and K2S2O8, in an air environment, irradiating with a 35 W blue LED light source and stirring at room temperature for 12 hours, after the reaction is completed, reducing pressure to remove a solvent, and then performing silica gel column chromatography on a crude product to obtain a product, namely the isoxazoline compound. The synthesis method provided by the invention avoids the problem of residue of a traditional metal catalyst, and provides a new normal form for green synthesis of the isoxazoline compound. As a key intermediate, isoxazoline can derive beta-lactam, beta-amino alcohol and other structures, and a new path is provided for complex molecule synthesis.

This invention provides a continuous process for producing ultrafine sodium azide, employing either System A or System B, including a nitrite ester synthesis section, a sodium azide synthesis section, and a gravity separation section. In the nitrite ester synthesis section of System A, the reaction temperature is -5℃ to 55℃, and the pressure is atmospheric pressure; the raw material alcohol includes methanol or ethanol. In the nitrite ester synthesis section of System B, the reaction temperature is -15℃ to 5℃, the pressure is atmospheric pressure, and the separation temperature is -5℃ to 55℃; the raw material alcohol includes methanol, ethanol, propanol, or isopropanol. This invention effectively enhances the mixing and transfer of materials under strong centrifugal force, thereby accelerating the reaction and separation speed. Even the azide reaction can proceed rapidly in the aqueous phase without a phase-transfer catalyst, reducing the reaction time from several hours to minutes. The residence time of materials in the equipment is extremely short, significantly shortening the production cycle.

The invention provides a preparation method of 2, 6-diaminobenzene, and relates to the technical field of organic synthesis. The preparation method comprises the following steps: taking 2-amino-4-nitrobenzoic acid as an initial raw material, carrying out diazotization reaction on the initial raw material and nitrite ester under an acidic condition, then carrying out cyclization reaction, and reducing by using a reducing agent to obtain the 2, 6-diaminobenzene. The preparation method provided by the invention is short in reaction route, high in atom conversion rate, high in product yield, high in production efficiency, simple to operate, cheap and easily available in raw material 2-amino-4-nitrobenzoic acid, low in production cost, green and environment-friendly, and suitable for industrial production. The preparation method provided by the invention has important significance on organic synthesis, medicinal chemistry and material chemistry of the biphenyl alkene derivative. The test result of the embodiment shows that the total yield of the 2, 6-diaminobenzene prepared by the preparation method provided by the invention is more than 43.9%.

The invention belongs to the field of medicine synthesis, and particularly relates to a preparation method of Remetirom (Remetirom). The preparation method comprises the following steps: reacting 2, 3, 6-dichloropyridazine, isobutyric acid, a catalyst, acid and a free radical initiator in a solvent to obtain an intermediate I; reacting the intermediate I with 4-amino-2, 6-dichlorophenol under the conditions of inert gas protection, catalyst and alkalinity to obtain an intermediate II; reacting the intermediate II with nitrous acid ester and N-cyanoacetyl ethyl carbamate under an acidic condition to obtain an intermediate III; and the intermediate III is subjected to a one-pot self-reaction in a carboxylate-carboxylic acid solvent to obtain the remetirol. The method provided by the invention has the advantages of short steps, low cost, mild reaction conditions, high total yield, suitability for industrial production and the like.

The invention discloses 4-bromo-2, 6-dimethyl fluorobenzene and a preparation method thereof, and belongs to the technical field of organic synthesis. The method provided by the invention comprises the following steps: reacting 4-bromo-2, 6-dimethylaniline, a boron trifluoride ether complex and nitrite ester in a reaction system in the presence of an organic solvent at the temperature of 75-105 DEG C to obtain a material containing 4-bromo-2, 6-dimethyl fluorobenzene; wherein the weight ratio of the 4-bromine-2, 6-dimethylaniline to the boron trifluoride ether complex to the nitrite ester is 1: (0.93 to 1.75): (0.58 to 0.88). According to the reaction method, an unstable intermediate fluoborate does not need to be separated, the safety is high, the large-scale production yield is stable, the purity is high, and the amount of three wastes is low.

The invention relates to the technical field of chemistry and chemical engineering, in particular to a method for efficiently preparing fluorene derivatives through a ball milling method. The method comprises the following steps: under the protection of an inert gas atmosphere, carrying out a ball-milling reaction on raw materials including 2-amino-2 '-iodobiphenyl, tert-butyl nitrite, a 1, 3-dicarbonyl derivative, palladium trifluoroacetate and potassium carbonate to obtain the 9, 9-disubstituted fluorene derivative as shown in a formula I. The invention provides a method for efficiently preparing the fluorene derivative through a ball-milling method. The preparation method can solve the technical problem that the preparation method of the organic photoelectric material containing the fluorene unit in the prior art is tedious and complicated in multiple steps, and has the characteristics of simplicity, high efficiency and environmental protection.

The application relates to the technical field of nitrite synthesis, and discloses a synthesis method and a synthesis device of alkyl nitrite. The synthesis method comprises the following steps: firstly, mixing gaseous nitric oxide and gaseous oxygen to obtain a mixture through a first reaction; and then, mixing the mixture with alkyl alcohol to obtain alkyl nitrite through a second reaction. The synthesis method greatly shortens the reaction time, increases the yield of alkyl nitrite, does not have a complicated post-treatment process and a large amount of by-product nitric acid, and is beneficial to cost saving and time saving.

The invention relates to the technical field of lithium ion batteries, in particular to a lithium ion battery electrolyte, a secondary battery, a battery module, a battery pack and an electric device. The lithium ion battery electrolyte comprises a lithium salt, an organic solvent and an additive, the additive comprises a compound shown as a formula (I), R1 to R4 are independently selected from a hydrogen atom, a halogen atom, a nitrate group, a nitrite group, a substituted or unsubstituted C1-12 alkyl group and a substituted or unsubstituted C1-12 alkoxy group, and the condition is that at least one of R1 to R4 is the nitrate group. The problems that an existing additive is poor in solubility, and the conductivity of formed SEI is not high are solved. # imgabs0 #

A synthesis method for sodium azide, comprising: using an aromatic alcohol as a raw material to prepare an alkyl nitrite of the aromatic alcohol; under alkaline conditions, reacting the alkyl nitrite with a hydrazine hydrate in a reduction reaction, to prepare sodium azide, the aromatic alcohol comprising one or more compounds having the structural formula represented as: (I), Ar being selected from any one of the following: substituted or unsubstituted C6-C20 aryl groups, and substituted or unsubstituted C3-C10 heteroaryl groups, R being selected from (II) and n being an integer of 1-3; in (III), R1 and R2 are the same or different, and are independently selected from any one of H and C1-C3 alkyl groups; when Ar is selected from substituted C6-C20 aryl groups or substituted C3-C10 heteroaryl groups, substituents of the substituted groups are selected from C1-C9 alkyl groups, and * represents a connection site.

The present invention relates to a method for synthesizing methyl 2-methyl-α-methoxyiminophenylacetate, belonging to the technical field of organic synthesis. The method process includes the following steps: Step1: Add o-halotoluene, methyl 2-(methoxyimino)acetate and a solvent into a reaction flask. X in the o-halotoluene is chlorine, and the solvent is toluene. Add a base and a catalyst. The base is sodium carbonate or potassium carbonate, and the catalyst is a Cu-TMEDA catalyst. After adding, keep the reaction at a certain temperature; Step2: After the reaction is completed, add water for washing, and concentrate the organic phase under reduced pressure to recover the solvent to obtain methyl 2-methyl-α-methoxyiminophenylacetate. The present invention uses o-halotoluene and methyl 2-(methoxyimino)acetate as raw materials to catalytically synthesize methyl 2-methyl-α-methoxyiminophenylacetate. Compared with the traditional synthesis process, it avoids the use of flammable and explosive nitrites, the reaction is safe and reliable, the raw materials are cheap and easily available, the process is simple and smooth, the reaction conditions are mild, and it is more suitable for industrial scale-up production.

This invention belongs to the field of organic synthesis, specifically relating to a green and efficient synthesis method for m-trifluoromethylacetophenone oxime. The specific steps are as follows: first, m-trifluoromethylaniline is added to a nonpolar solvent and reacts with nitrite ester under the action of an organic acid to generate a diazonium salt. Then, under the combined action of a phase transfer catalyst and a copper salt catalyst, it reacts with acetaldehyde oxime to generate m-trifluoromethylacetophenone oxime. After heating and filtering the copper salt catalyst, the mixture is cooled and crystallized to obtain m-trifluoromethylacetophenone oxime with a content of over 98% and a yield of over 90% based on m-trifluoromethylaniline. The above synthesis method generates less waste, has high atom utilization, high reaction yield, simple operation, strong process stability, and is easy for industrial production.

The invention relates to a synthetic method of 2-methyl-alpha-methoxyimino methyl phenylacetate, and belongs to the technical field of organic synthesis, the process of the method comprises the following steps: Step 1: adding o-halotoluene, 2-(methoxyimino) methyl acetate and a solvent into a reaction flask, adding alkali and a catalyst, reacting for 1-2 hours at the temperature of 50-60 DEG C, and reacting for 1-2 hours to obtain 2-methyl-alpha-methoxyimino methyl phenylacetate; the alkali is sodium carbonate or potassium carbonate, and the catalyst is a Cu-TMEDA catalyst; 2, after the reaction is finished, water is added for washing, an organic phase is concentrated under reduced pressure, the solvent is recycled, and 2-methyl-alpha-methoxyimino methyl phenylacetate is obtained. The 2-methyl-alpha-methoxyimino methyl phenylacetate is obtained through catalytic synthesis by taking o-halogen toluene and 2-(methoxyimino) methyl acetate as raw materials, compared with a traditional synthesis process, flammable and explosive nitrite ester is not used, the reaction is safe and reliable, the raw materials are cheap and easy to obtain, the process is simple and smooth, the reaction conditions are mild, and the method is suitable for industrial production. The method is more suitable for industrial large-scale production.

The invention discloses a continuous production method of (E) 2-hydroxyimino-[(2-o-methylphenyl)] acetic acid, and belongs to the field of organic synthesis industrial products.The continuous production method of (E) 2-hydroxyimino-[(2-o-methylphenyl)] acetic acid comprises the following steps that a compound o-methylphenylacetonitrile shown in the formula I is used as a raw material, a reaction is carried out for 2-4 hours, and a reaction solution is obtained; continuously reacting the (E)-2-hydroxyimino-[(2-o-methylphenyl)] acetic acid with nitrite and alkali according to a certain proportion through series connection of three stages of reaction kettles, continuously flowing the obtained reaction liquid into an acidification kettle, adding acid for acidification reaction, and centrifugally drying to obtain (E)-2-hydroxyimino-[(2-o-methylphenyl)] acetic acid; wherein the R group of the nitrous acid ester is an alkyl group and is independently selected from tertiary butyl, n-butyl, ethyl, n-propyl or isopropyl. The synthesis method is low in reaction cost, high in production efficiency, stable in product quality and suitable for industrial production.

The invention discloses a cyclic regeneration method of a catalyst for preparing a 3, 3-dialkoxy propyl compound, which comprises the following steps: reacting an allyl compound with nitrite under the action of the catalyst, adding a reducing agent into the reaction system after the reaction is finished, filtering, and continuously rectifying the filtrate to obtain the 3, 3-dialkoxy propyl compound. The filter residues are oxidized by an oxidizing agent under the action of acid to generate a catalyst, and the catalyst is a bivalent palladium catalyst or a mixture of the bivalent palladium catalyst and a bivalent copper catalyst. An oxidizing agent and a reducing agent are added into a reaction system, so that the conversion of deactivation and reactivation of the catalyst is realized, coordination ions of the catalyst are provided by acid, and the cyclic regeneration of the catalyst is realized under the action of the oxidizing agent.

The invention provides a pyrone compound and a preparation method and application thereof, and belongs to the field of pharmaceutical chemicals, the preparation method comprises the following steps: carrying out aldoxime hydrolysis or oxidation on a product generated by oximation of 3-(benzyloxy)-2-methyl-4H-pyran-4-ketone and nitrite ester to form aldehyde, oxidizing the aldehyde into acid, and carrying out acid hydrolysis or oxidation on the acid to obtain a pyrone compound; the important intermediate 3-(benzyloxy)-4-oxo-4H-pyran-2-carboxylic acid in the field of pharmaceutical and chemical engineering is obtained. The product obtained by the method disclosed by the invention is high in purity and high in yield; the method disclosed by the invention has the characteristics of low total cost, simplicity in operation and stable process.

The invention belongs to the field of chemical synthesis, and particularly relates to a synthetic method of m-trifluoromethyl acetophenone, which comprises the following steps: 1, preparing nitrite through nitrosation reaction, 2, simultaneously dropwise adding the nitrite and m-trifluoromethyl aniline into an acetic anhydride substrate for reaction to directly obtain a product m-trifluoromethyl acetophenone feed liquid, and 3, carrying out post-treatment to obtain the m-trifluoromethyl acetophenone. And washing and rectifying to obtain the product. According to the scheme, the process route of preparing the m-trifluoromethyl acetophenone through diazotization, coupling and acidolysis reaction in the traditional process is broken through, the nitrite and the m-trifluoromethyl aniline react with the acetic anhydride under the action of the catalyst to directly synthesize the m-trifluoromethyl acetophenone in one step, the reaction steps are shortened, the generation of wastewater is greatly reduced, and the production cost is reduced. And the effect of reducing the cost is achieved.

The invention provides an amplified preparation method of a key intermediate of an estrogen receptor modulator, and belongs to the field of medical intermediates. The method comprises the following steps: by taking azetidine-3-one hydrochloride and 3-fluoro-1-halogenated propane as raw materials, reacting in the presence of alkali to obtain an intermediate 1; then carrying out reductive amination reaction on the intermediate 2 and 5-amino-2-methylpyridine to obtain an intermediate 2; reacting with nitrous acid ester in the presence of alkali to obtain an intermediate 3; and finally, reacting in the presence of acid to obtain the 5-((1-(3-fluoropropyl) azetidine-3-yl) amino) pyridinealdehydes. The method is simple and reliable in process and easy for industrial production; the generation amount of an isomer is reduced, and the reaction yield is improved.

The invention relates to a synthetic method of 2, 6-diethyl-4-methyl bromobenzene, which specifically comprises the following steps: reacting 2, 6-diethyl-4-methylaniline hydrobromide with phosphorus pentoxide and alkyl nitrite in the presence of an organic solvent. According to the method disclosed by the invention, water in the system can be fully removed, the generation of hydrolysis side reaction is avoided, the content of phenol impurities is reduced, meanwhile, the bromination reaction balance can be shifted rightwards, the bromination reaction yield is improved, and the production cost is greatly reduced. In addition, an alkali washing impurity removal step in an existing post-treatment procedure is avoided, impurities can be fully removed through simplified operation, the discharge amount of three wastes is reduced, and industrial production is facilitated.

This application relates to the technical field of lithium-ion batteries, in particular to a lithium-ion battery electrolyte solution, a secondary battery, a battery module, a battery pack, and an electrical device. The lithium-ion battery electrolyte solution includes a lithium salt, an organic solvent and an additive. The additive includes acompound represented by Formula I: where R1 to R4 are each independently selected from a hydrogen atom, a halogen atom, a nitrate ester group, a nitrite ester group, a substituted or unsubstituted C1 to C12 alkyl, and a substituted or unsubstituted C1 to C12 alkoxy, provided that at least one of R1 to R4 is a nitrate ester group. This application solves the problems of poor solubility of existing additives and low conductivity of a formed solid electrolyte interphase (SEI).

The present invention relates to a novel method of synthesizing mononitrosylated and dinitrosylated propanediols and novel compositions and pharmaceutical formulations comprising said compounds. The method is carried out by reacting the corresponding non-nitrosylated propanediol with a source of nitrite, optionally in the presence of a suitable acid. Therein, when the source of nitrite is an organic nitrite, the reaction step is performed in a suitable organic solvent and when the source of nitrite is an inorganic nitrite, the reaction step is performed in a biphasic solvent mixture comprising an aqueous phase and a non-aqueous phase. The present invention further relates to methods of treating conditions in which the administration of nitric oxide (NO) has a beneficial effect, by administering said compounds, compositions or formulations.

The invention discloses a multilayer nested efficient nitrite separation tower structure, which comprises a tower body, the tower body is sequentially divided into an absorption section, a reaction section and a rectification section from top to bottom, and the sections are nested and connected through an annular support frame to form a continuous gas-liquid mass transfer channel; the absorption section is positioned at the top of the tower body, is filled with high-porosity metal foam filler and is provided with a first inlet for fresh alkyl alcohol; the reaction section is located in the middle of the tower body and divided into an upper layer and a lower layer, the upper layer is filled with regular ceramic corrugated filler and provided with a second inlet containing nitric oxide and oxygen, and the lower layer is filled with wire mesh filler; the rectifying section is positioned at the bottom of the tower body, filled with molecular sieve particles and provided with a third inlet containing nitrogen oxide and an evaporator; the height ratio of the absorption section to the reaction section to the rectifying section is (2-6): (3-8): 1. By designing the multi-layer nested high-efficiency nitrite ester separation tower, the problems of flow simplification and comprehensive efficiency improvement in nitrite ester production are adaptively solved.

The invention relates to the technical field of synthetic chemistry, in particular to a method for preparing 4-bromo-3-methoxyphenol. Comprising the following steps: (1) hydrolyzing a compound of formula I to generate a compound II; (2) reacting the compound shown in the formula II with toluene-4-sulfonyl chloride to generate a compound III; (3) reducing the compound in the formula III to generate a compound IV; (4) reacting the compound shown in the formula IV with nitrite or nitrite ester, and then reacting with a bromination reagent to generate a compound V; and (5) hydrolyzing the compound of formula V to generate a compound VI. According to the preparation method provided by the invention, the target product 4-bromo-3-methoxyphenol is efficiently prepared under mild conditions through the reaction steps of hydrolysis, substitution, reduction, bromination and the like, so that the problems of harsh oxidation reaction conditions, no reaction selectivity concern and high total molar yield of the original process are avoided, and the preparation method has the advantages of more controllable quality, high atom economy, low cost and the like. The process is stable, and production is easy. The synthesis route is shown in the specification.

Described is a process for the synthesis of mono- and bis-nitrosylated propanediols, as well as compositions and pharmaceutical formulations that includes the compounds. The process proceeds by reacting a corresponding propanediol that is not nitrosylated with a source of nitrite, optionally in the presence of a suitable acid. When the source of nitrite is an organic nitrite, reacting step is performed in a suitable organic solvent, and when the source of nitrite is an inorganic nitrite, the reacting step is performed in a bi-phasic solvent mixture comprising an aqueous phase and a non-aqueous phase. Also disclosed are methods of treating a condition wherein administration of nitric oxide (NO) has a beneficial effect by administering said compounds, compositions or formulations.