63 results about "Butyl nitrite" patented technology

The invention discloses a synthesis method of a 1,2,3-diazosulfide compound. A o-aminothiophenol compound with a structure shown as a formula (I) and tert-butyl nitrite are taken as raw materials, and are subjected to intramolecular diazo-reaction to obtain the 1,2,3-diazosulfide compound with a structure shown as a formula (II); a reaction equation is as follows (shown in the description), wherein R=hydrogen, fluorine, chlorine, ester group, nitro or methyl. The synthesis method has the beneficial effects that (1) the operation is simple and convenient in a preparation process, an obtained product is easy for after-treatment, and large-scale industrialized production is suitable; (2) reaction conditions are mild; (3) the synthesis cost is lowered; (4) a reaction substrate is high in functional group tolerance, is wide in range and easy to prepare; (5) the reaction is efficient, the yield is high, and the reaction efficiency is higher after reaction amplification; (6) environment pollution is avoided, and environment friendliness is achieved.

A disclosed preparation method for erythro-structure methoxamine hydrochloride comprises the following steps: (1) dissolving an initial raw material 2,5-dimethylpropiophenone in an organic solvent, under the condition of introducing dry hydrogen chloride gas, dropwise adding a 1-butyl nitrite solution to perform an oximation reaction, so as to obtain an intermediate I; (2) under the acidic condition, taking a methanol solution as a solvent, take palladium on activated carbon as a catalyst, employing hydrogen to reduce the oximido group in the intermediate I, so as to obtain an intermediate II; and (3) performing hydrogenation reduction reaction on the intermediate II to obtain the erythro-structure methoxamine hydrochloride. The method provided by the invention is simple in operation, economic, environment-friendly, mild in reaction conditions, excellent in product quality and high in yield, and can help to obtain the single erythro-structure methoxamine hydrochloride.

The invention relates to a hydrogen sulfide fluorescent probe as well as preparation and application thereof. The molecular formula of the fluorescent probe is C27H25NO9; the preparation method of thefluorescent probe comprises the following steps: reacting a fluorescein with sodium hydroxide; reacting an obtained product with 2-(2-(2-methoxyethoxy)ethoxy)ethyl 4-methylbenzenesulfonate to obtaina compound 4, reacting the compound 4 with N-Phenylbis(trifluoromethanesulphonimide) to obtain a compound 3, reacting the compound 3 with bis (pinacolato) diboron to obtain a compound 2, hydrolyzing the compound 2, and reacting an obtained product with tert-butyl nitrite to obtain the hydrogen sulfide fluorescent probe. The probe shows relatively high selectivity on detection of hydrogen sulfide in a pure water solution.

The invention provides a method for preparing a chiral 3-nitroindole compound through a nickel-catalyzed asymmetric nitration reaction. The method comprises the following steps: in a solvent, under the action of an additive, a nickel catalyst and a ligand, carrying out an asymmetric nitration reaction on an indole-2-one compound I and tert-butyl nitrite II to obtain the chiral 3-nitroindole compound III. According to the invention, chiral 3-nitroindole is constructed through a nickel-catalyzed asymmetric nitration reaction, and the method has the advantages of low catalyst cost, convenience in operation, wide substrate application range, cheap and easily available reaction raw materials and the like.

The invention discloses a synthesis method of a 1,2,3-phentriazine-4(3H)-one compound. 2-aminobenzamide and are used as raw materials and tert-butyl nitrite stirred at the room temperature in a reaction solvent, and the 1,2,3-phentriazine-4(3H)-one compound is obtained through an intramolecular diazotization reaction. The reaction equation is shown in the description, wherein R is H, fluorine, chlorine, bromine, trifluoromethyl, nitryl or methyl. The synthesis method has the benefits as follows: (1) the synthesis method is convenient in experiment operation, easy in posttreatment, mild in reaction condition and suitable of large-scale industrial production; (2) reaction substrate functional groups have high tolerance, and the substrate is wide in range and easy to obtain; (3) the reactionefficiency, yield and purity are higher.

The invention discloses a preparation method of a quinoxalin-2-one derivative and a product purification method. The preparation method comprises the following steps: using N-methyl-N-phenyltrifluoropropionamide or its derivative as a substrate, adding tert-butyl nitrite into the substrate, using an acetonitrile solution as a solvent, and heating to carry out a reaction in the environment of a buffer solution prepared from a 4 Angstrom molecular sieve, cesium carbonate and acetic acid so as to prepare a crude product. Then, the crude product undergoes purification. The purification method comprises the following steps: filtering the crude product and removing acid to obtain residue; carrying out silica-gel column chromatography on the residue, leaching with an eluate and collecting an eluant; merging product-containing eluants; condensing the merged eluant to remove the solvent; and finally carrying out vacuum drying to obtain a target product. The invention has advantages of simple technological process, low cost and high yield.

The invention belongs to the technical field of medicine synthesis, and in particular relates to a method for synthesizing a Crizotinib intermediate. The method comprises steps of: a) reacting a raw material 4-mesylate piperidine-1-formic acid tert-butyl ester (2) with 4-nitro pyrazole to prepare a compound 3; b) reducing nitro by using hydrazine hydrate to obtain an amino compound 4; and c) diazotizing the compound 4 by using tert-butyl nitrite, and reacting the compound 4 with a boric acid ester compound 5 in the presence of a free radical initiator benzoyl peroxide, so as to prepare the Crizotinib intermediate (1). Compared with an existing synthesis method, the method provided by the invention has the following advantages: a diazotization method is used to synthesize the boric acid ester product; and compared with an existing Miyaura boronation method catalyzed by Pd, the method avoids the usage of expensive palladium catalyst and ligand, and has the merits of mild reaction condition, high yield, simple operation, cheap and easily available raw materials and short reaction period, and is quite easy for industrialized mass production.

The invention provides a method for preparing aromatic hydrocarbon alpha ketone carbonyl compounds through continuous visible light catalytic molecular oxygen oxidation in a micro-channel reactor, andbelongs to the technical field of continuous flow photocatalytic synthesis. According to the method, molecular oxygen is used as an oxidizing agent, N-hydroxyphthalimide and tert-butyl nitrite are used as catalysts, and isobutylbenzene is used for preparing isobutyryl benzene under the condition of visible light. The product isobutyryl benzene has photosensitive activity, the catalytic reaction is carried out under visible light, and the highest yield of the obtained isobutyryl benzene can reach 86.3%. The reaction conditions are mild, the isobutyryl benzene can be efficiently prepared without additional metal, alkali and the like, and the operation is simple. With application of the micro-channel reactor, the reaction time is greatly shortened, the mass and heat transfer efficiency is obviously improved, the energy consumption is reduced, and three-waste emission is reduced.

The invention discloses a photocatalytic oxidation synthesis method of a benzocoumarin compound. A 2-aryl-aryl formic acid compound is used as a reaction raw material; 2,3-dichloro-5,6-dinitrile-1,4-benzoquinone (DDQ) and tert-butyl nitrite (TBN) are used as catalysts, oxygen is used as an oxidant, a reaction substrate is subjected to a reaction in an organic solvent under the conditions of normaltemperature, normal pressure and blue light irradiation, and after the reaction is finished, separation treatment is performed to obtain the benzocoumarin compound. Compared with a traditional heating reaction, the synthesis method provided by the invention has the advantages that the illumination reaction can save energy; oxygen is used as a terminal oxidant, so that the environmental cost is reduced; a transition metal catalyst is not used, so that the problem of metal residues in the product can be solved.

The invention discloses a simple preparation method of isoxazoline. The simple preparation method is characterized in that a series of isoxazoline compounds are efficiently synthesized by using aldehyde, p-toluenesulfonhydrazide, olefin and tert-butyl nitrite as substrates, copper chloride as a catalyst and tetramethylethylenediamine (TMEDA) as alkali through the one-pot two-step method. The method has the advantages that the catalyst is cheap, reaction is economical, good substrate universality is achieved, the raw materials are easy to obtain, later-stage functionalization is more convenient, reaction conditions are mild, and gram-level scale reaction is good; and especially, the compounds with medium yield can be obtained without the catalyst, post-treatment is simple and convenient, the application of the compoumds in drug molecule synthesis and large-scale industrialization is facilitated, and the requirements and trends of modern green chemistry and medicinal chemistry are met.

The invention belongs to the field of organic synthesis, and specifically discloses a preparation method of alpha-nitro ketoxime derivatives. The method comprises the steps of taking a styrene derivative of the formula I-1 as a reaction raw material and butyl nitrite as a nitration reagent, adding an assistant, and reacting with water as a solvent under the condition of air at room temperature to obtain the alpha-nitro ketoxime derivative of formula I, has the characteristics of low production cost, mild process conditions, high yield, and environmentally friendly effects, and is very suitable for industrial production. The reaction formula of the method is shown in the description.

The invention discloses a preparation method of a polysubstituted pyrroline compound, and belongs to the technical field of fine chemical engineering. According to the method, N-2-methylallyl-N-3-arylpropargyl p-toluenesulfonamide is used as a raw material, a specific ferric salt is used as a catalyst, tert-butyl nitrite is used as an oxidizing agent, polymethylsiloxane (PMHS) is used as a hydrogen source, and a reaction is carried out in an inert atmosphere; and then a reaction is performed in an I2 / H2O2 system to synthesize a target product, namely the polysubstituted pyrroline compound. The method has the advantages of cheap catalyst, mild reaction condition and the like, and has a good application prospect.

The invention discloses a sound-insulation and heat-insulation hollow-glass spacing bar. The sound-insulation and heat-insulation hollow-glass spacing bar is prepared from, by weight, 14-18 parts of polydimethylsiloxane, 5-10 parts of hexamethyldisiloxane, 4-9 parts of ring methyl siloxane, 4-9 parts of vinyltriethoxysilane, 4-7 parts of sodium acrylate, 3-6 parts of butyl nitrite, 2-7 parts of ethyl chloroformate, 5-11 parts of white carbon black, 4-6 parts of isoamyl chloride, 5-7 parts of 3-hydroxy-2-butanone, 2-3 parts of sodium hydrogen sulfite, 4-8 parts of maleic anhydride, 1-3 parts of benzoyl chloride, 2-3 parts of copper chloride, 1-4 parts of sulfamic acid, 3-5 parts of sodium ethoxide, 5-8 parts of a crosslinking agent and 4-6 parts of a thickening agent. The sound-insulation and heat-insulation hollow-glass spacing bar is good in sound insulation and heat insulation. In addition, the invention further discloses a relevant preparation method.

The invention discloses a sodium alginate-based nitric oxide donor as well as a synthesis method and application thereof. The synthesis method comprises the following steps: dissolving sodium alginate in ultrapure water, adding an activating agent for reaction, adding L-cysteine hydrochloride or cystamine dihydrochloride for continuous reaction; and dialyzing the reaction solution, adding tert-butyl nitrite, continuously reacting, dialyzing the obtained solution, and freeze-drying to obtain the sodium alginate nitric oxide donor. The sodium alginate nitric oxide donor synthesized by the method is S-nitrosylated sodium alginate, sulfydryl is grafted on sodium alginate, SNO groups are formed through nitrosation, the synthesis method is simple and easy to implement, non-toxic and low in cost, and the prepared nitric oxide donor is long in release time, can exist stably, and can be used for preparing the sodium alginate nitric oxide donor. And the material and other polymer materials are expected to be applied to preparation of multifunctional nitric oxide release composite materials.

The invention relates to the technical field of synthetic rubber, and discloses rubber containing modified graphene, which comprises the following components: rubber, carbon black, zinc oxide, stearic acid, sulfur, an accelerant, a scorch retarder and modified graphene. The modified graphene is obtained by fully mixing and ball-milling graphite and a modifier, then adding tert-butyl nitrite and a solvent, mixing and ball-milling, fully mixing, washing and drying; and the modifying agent is one or more of amino propionyl aniline, 4-aminobenzoyl aniline, 2-amino-N-cyclohexyl-N-methyl benzene methylamine, 4-(4-isopropyl piperazine-1-yl) aniline, (4-aminobenzene)-4-(4-methoxyphenyl) piperazine, (4-(4-aminobenzyl) piperazine-1-yl) ethanone and (4-aminobenzene)-4-(4-methoxyphenyl) piperazine. Rubber formed by mixing and refining the modified graphene and other components of rubber has a better anti-aging effect.

The invention relates to a synthesizing method of novel chiral nitro binaphthol and derivatives thereof, and belongs to the field of organic synthesis. A novel green free radical nitrifying method isprovided, and comprises the following steps of using chiral binaphthol as the raw material, and generating free radical nitrifying reaction with a green nitrifying reagent (TBN (tert-butyl nitrite)) at room temperature by using tetrahydrofuran as a reaction solvent, so as to obtain the chiral nitro binaphthol. The synthesizing method has the advantages that the metal is not used in reaction, and the TBN is directly used in the nitrifying reaction; only the product and tertiary butanol are generated in reaction, and the pollution to environment is reduced; the important application prospect isrealized in the synthesizing field of the chiral nitro binaphthol, the green nitrifying is truly realized, and a novel concept is provided for the large-scale industrialized production of the nitro binaphthol.

The invention belongs to the field of organic synthesis and azo dyes and particularly discloses an imidazo heterocyclic azo derivative and a preparation method and application thereof. The imidazo heterocyclic azo derivative has a structural formula shown as in formula (1), wherein heterocyclic Het is one of pyridine, thiazole and pyrimidine; R is C1-C6 alkyl groups, or aryl groups containing F, Cl, Br, MeO, CN and NO2 or aryl groups that are acetyl-substituted; Ar is aryl groups containing F, Cl, Br, MeO, CN and NO2 or aryl groups that are acetyl-substituted. The preparation method of the invention is an economical, simple and environment-friendly green synthetic method, neither the addition of mass hydrochloric acid or sulfuric acid and nitrites nor the pre-preparation of diazonium salts is required in the method, and imidazo heterocyclic azo compounds are directly produced under the action of tert-butyl nitrites. The imidazo heterocyclic azo derivative prepared herein has good fluorescent properties and is useful in the fields such as fluorescent dyes, luminescent materials and bactericides.

The invention discloses a preparation method of 1-(tert-butyl)-3-chloronaphthalene. The preparation method comprises the following steps: reacting 1-naphthylamine with N-chlorosuccinimide in a solvent to generate a first intermediate; reacting the first intermediate with N-bromosuccinimide in a solvent to generate a second intermediate; reacting a first reaction system containing the second intermediate, lewis acid, tert-butyl nitrite and a solvent, and then adding hypophosphorous acid and cuprous oxide into the first reaction system for reaction to generate a third intermediate; and reacting a second reaction system containing a catalyst ligand, nickel acetylacetonate, lithium tert-butoxide, isopropyl magnesium chloride and a solvent in a protective atmosphere, and then adding the third intermediate into the second reaction system for reaction to generate 1-(tert-butyl)-3-chloronaphthalene. The preparation method disclosed by the invention is short in process route, simple to operate, mild in condition, environment-friendly, low in cost, high in target product yield, few in by-products and beneficial to industrial production.

The invention relates to a method for preparing isoxazoline, which comprises the steps of reacting olefin, a diazo compound and tert-butyl nitrite in an organic solvent at the temperature of 25-50 DEGC under the action of a Lewis acid catalyst to obtain isoxazoline after complete reaction. Lewis acid is used as a catalyst for synthesizing isoxazoline, reaction conditions are mild and can be carried out under the condition that the temperature is as low as the room temperature, use of transition metal is avoided, and the product yield is high.

The invention discloses a synthesis method of 2-(2-methoxy-4-nitrophenyl)-3-(4-nitrophenyl)-5-(2,4-disulfophenyl)-2H-tetrazole monosodium salt (WST-8), belonging to the technical field of chemical synthesis. According to the synthesis method, the raw materials benzaldehyde-2,4-sodium disulfonate and p-nitrophenylhydrazine are subjected to four-step reaction by using N-bromosuccinimide (NBS) as an oxidizer, thereby obtaining the WST-8. The invention is safe and simple to operate and easy for after-treatment, and avoids using chlorine gas, n-butyl nitrite and other high-toxicity high-price compounds; and the total yield of the four-step reaction is up to 34.4%, thereby being beneficial to industrial production.

The invention discloses a chromium-containing waste leather scrap treatment method. The method comprises the following steps: carrying out hydrolysis treatment on chromium-containing waste leather scraps serving as a raw material, and carrying out enzyme hydrolysis on the chromium-containing waste leather scraps by using protease; carrying out further hydrolysis on the chromium-containing waste leather scraps by using an acid solution to hydrolyze the chromium-containing waste scraps into collagen polypeptide molecules, wherein the acid solution is a mixture of an aqueous sulfuric acid solution and an aqueous lactic acid solution; then modifying the collagen polypeptide molecules with a modifier, wherein the modifier is consisting mixture of of 2,3-pyridinedioic anhydride, 7-chloro-2H-benzo[e][1,2,3,4]thiatriazine-1,1-dioxide and 4,4'-diamino-3,3'-biphenyl disulfonic acid, wherein the 7-chloro-2H-benzo[e][1,2,3,4]thiatriazine-1,1-dioxide is obtained by reacting 2-amino-5-chlorobenzenesulfonamide with tert-butyl nitrite; and performing treatment to process the chromium-containing waste leather scraps into a retanning filler. The retanning filler has a good tanning and retanning filling effect, and tanned leather is full, soft, good in elasticity and clear and fine in grain.

The invention discloses a preparing method of a heterocyclic urea indoleamine-2-3-dioxygenase enzyme inhibitor intermediate. Malononitrile and hydroxylamine hydrochloride serve as raw materials, and 3-amino-4-aminoxime furza is obtained through a sodium nitrite reaction; afterwards, benzophenone is adopted for amino protection, and then 3-amino-4-aminoxime furza is reacted with 3-bromine-4-fluoroaniline after being diazotized with tert-butyl nitrite to obtain 4-diphenyl agag amino-N-(3-bromine-4-fluorophenyl)-N'-hydroxy-1,2,5-oxadizole-3-formamidine; after protection of carbonic ester ring closure and benzophenone, the heterocyclic urea indole amines-2-3-dioxygenase enzyme inhibitor intermediate, namely 3-(4-amino-1,2,5-oxadiazole-3-radical)-4-(3-bromine-4-fluorophenyl)-1,2,4-oxidazole-5(4H)-ketone is generated. The preparing method is high in reaction yield, convenient to operate, low in cost and suitable for industrialized production.

The invention discloses a method for synthesizing an aromatic trifluoromethylthio compound. The method comprises the following steps: reacting sodium trifluoromethanesulfinate with Chlorodiphenyl phosphine at room temperature; after reacting for a period of time, sequentially adding an aniline compound and tert-butyl nitrite, fully reacting at 70 + / -5 DEG C by taking CuSO4 as a catalyst and acetonitrile as a solvent, cooling to room temperature after the reaction is finished, extracting, carrying out reduced pressure distillation, and carrying out column chromatography separation and purification on the reaction mixture to obtain the aromatic trifluoromethylthio compound. The method is simple and safe in process operation and high in reaction conversion rate, the used raw materials are economical and practical, few three wastes are generated, and no extra organic solvent needs to be treated.

The invention belongs to the technical field of compound preparation, and particularly relates to a visible light mediated dihydroisoxazole synthesis method. Comprising the following steps: taking terminal olefin, a dibromomalonic acid compound and tert-butyl nitrite as raw materials, and carrying out cascade cyclization reaction in a solvent under the actions of argon protection, visible light, a photosensitizer and alkali to synthesize the dihydroisoxazole compound. The method is an effective method for constructing dihydroisoxazole through [2 + 2 + 1] intermolecular cyclization, the conditions are mild, and the three raw materials are easy to buy in the market and low in price.

The invention discloses a method for synthesizing aromatic fluoromethylthio compounds through a one-pot method. The method uses aromatic amines as raw materials, under the action of tert-butyl nitrite and tetrafluoroboric acid, with anhydrous acetonitrile as a solvent, first reacts in an ice bath to generate the corresponding diazonium salt; then reacts in copper chloride, chlorine Under the action of cuprous chloride and 1,10-phenanthroline, potassium thiocyanate was used as a sulfur source to react and introduce sulfur atoms in an ice bath; finally, under the action of potassium hydroxide, through a fluoroiodomethane, in an ice bath Introducing a fluoromethyl group in the reaction to obtain an aromatic fluoromethylthio compound. The method of the invention has simple and safe steps, high reaction conversion rate, less waste, and is environmentally friendly.

The invention discloses a photocatalytic oxidation synthesis method of diphenylmethanol ester. The method is characterized in that diphenylmethanol and carboxylic acid are used as reaction substrates,2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ) and tert-butyl nitrite (TBN) are used as a catalyst, and oxygen is used as an oxidant, in the presence of 3A or 4A molecular sieves, the reaction substrates react in the 1,2-dichloroethane solvent under conditions of room temperature, normal pressure and blue light irradiation, and after the reaction ends, a diphenylmethanol ester compound is obtained by separation treatment. According to the invention, by replacing the traditional heating reaction with light reaction, the energy is saved; and the reaction is environmentally friendly by using oxygen as the oxidant.

The invention relates to a method for preparing a benzimidazole [2, 1-a] isoquinoline-6 (5H)-ketone compound. The method comprises the following steps: adding an N-methylacryloyl-2-phenyl benzimidazole compound, a nitrile compound / acetone / tert-butyl nitrite, a catalyst, an oxidizing agent and a solvent into a Schlenk reaction flask, and stirring and reacting at a certain temperature in an air atmosphere to obtain the cyanogen-containing alkyl / ketone skeleton / nitro-substituted benzimidazole [2, 1-a] isoquinoline-6 (5H)-ketone compound.

The invention discloses a method for synthesizing aromatic trifluoromethylthio compounds. The steps are: under the protection of argon, react sodium trifluoromethanesulfinate and diphenylphosphorous chloride at room temperature; 4 As a catalyst, acetonitrile is used as a solvent to fully react at 70±5° C. After the reaction is completed, cool to room temperature, extract, and distill under reduced pressure. The reaction mixture is separated and purified by column chromatography to obtain the aromatic trifluoromethylthio compound. The process of the invention has simple and safe operation, high reaction conversion rate, economical and practical raw materials, less three wastes and no need to process additional organic solvents.

The invention provides a preparation method for naphthyl-1,8-diaminoarylboramide. The preparation method comprises the following steps: sequentially adding Bpin-Bdan, tetrabutylammonium iodide, sodiumacetate, dibenzoyl peroxide and tert-butyl nitrite into a reaction vessel, adding arylamine and acetonitrile in a nitrogen atmosphere, carrying out heating and vigorous stirring for a reaction, filtering an obtained reaction liquid, performing spin-drying of a solvent, and carrying out column chromatographic separation so as to obtain the target product. The method of the invention is quick and efficient in reaction, and functional groups have good tolerance and are compatible with halogen, ester groups, hydroxyl groups, cyano groups, amino groups and the like.