T:Toxic;
79-46-9Relevant articles and documents
Preparation method of nitro compound
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Paragraph 0046-0047; 0049-0050, (2021/03/13)
The invention discloses a preparation method of a nitro compound, which comprises: carrying out a reaction on a compound 1A and a compound 1B to obtain a compound 2A; and reacting the compound 2A witha nitration reagent to obtain a nitro compound crude product, and purifying to obtain a nitro compound fine product. According to the method, a reagent with low price is used as an initial raw material to prepare the final product through two-step reaction, wherein the reaction condition of each step is mild, the yield of the obtained nitro compound is high, and the cost can be greatly reduced.
Preparation method of nitroalkane compound
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Paragraph 0018; 0020; 0022; 0024; 0026; 0028; 0029; 0030, (2018/04/03)
The invention provides a preparation method of a nitroalkane compound and relates to the field of nitroalkane compounds. The preparation method comprises the following operations: mechanically stirring alkyl bromide, sodium nitrite, a catalyst, urea and a solvent at 50-60 DEG C, after carrying out a reaction for 5-6h, removing salts in a reaction solution by filtering, and then, removing an organic phase by reduced pressure distillation to obtain the nitroalkane compound, wherein the nitroalkane compound comprises the following components in parts by mole: 1 part of alkyl bromide, 1.2-2 partsof sodium nitrite, 0.01-0.3 part of catalyst and 0.005-0.5 part of urea; and the addition amount of the solvent is 1-2 times as much as the volume of alkyl bromide. According to the preparation method, urea is used as an additive to be introduced to a reaction of alkyl bromide and sodium nitrite, and with a reaction of 2-bromopropane and sodium nitrite as an example, it is unexpected that the reaction yield is increased to 85% or above and even higher than 97.4%, and therefore, the reaction yield is greatly increased; the preparation method is safe in operation, mild in reaction condition, lowin energy consumption and high in safety; and the preparation method is low in cost, extremely simple in aftertreatment and suitable for large-scale industrial production.
Green synthesis of low-carbon chain nitroalkanes via a novel tandem reaction of ketones catalyzed by TS-1
Chu, Qingyan,He, Guangke,Xi, Yang,Wang, Ping,Yu, Haoxuan,Liu, Rui,Zhu, Hongjun
, p. 46 - 50 (2018/02/09)
A green and efficient one-pot method has been developed for the synthesis of low-carbon chain nitroalkanes via a novel TS-1 catalyzed tandem oxidation of ketones with H2O2 and NH3. The tandem reaction including ammoxidation, oximation and oxidation of oximes, afforded up to 88% yield and 98% chemo-selectivity requiring only 90 min, at 70 °C and atmospheric pressure. Moreover, this method was even amenable to 100-fold scale-up without loss of chemical efficiency with 87% yield, represents a significant advance towards industrial production of nitroalkanes. Furthermore, the plausible mechanism of TS-1 catalyzed tandem oxidation of ketones to prepare nitroalkanes was proposed.
Green synthesis method for one-pot process preparation of AMP-95
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Paragraph 0033; 0035; 0037; 0039; 0041; 0043; 0045; 0046, (2018/07/07)
The invention discloses a green synthesis method for the one-pot process preparation of AMP-95. The method comprises the following steps: S1, preparing 2-nitropropane from acetone, hydrogen peroxide and ammonia in an alcohol solution under the catalysis of a catalyst; S2, directly reacting a reaction solution obtained in step S1 with formaldehyde or paraformaldehyde under an alkaline condition without purifying in order to generate 2-nitro-2-methyl-1-propanol; and S3, directly hydrogenating the reaction product obtained in step S2 without purifying to obtain the product 2-amino-2-methy-1-propanol (AMP-95), and rectifying the product to make the purity reach 99.5% or more. The method has the advantages of cheap and easily available raw materials, simple reaction steps, small pollution to the environment, low cost, high yield, easiness in purification of the product, and suitableness for industrial production.
Green synthesis method for preparing nitroalkanes by oxime oxidation
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Paragraph 0017; 0018, (2017/08/29)
The invention belongs to the field of organic chemical industries, and provides a green synthesis method for preparing nitroalkanes by oxime oxidation. At the temperature of 55 to 120 DEG C and under the pressure of 0 to 1.0 MPa, oxime, a solvent and hydrogen peroxide are reacted for 20 to 200min in the presence of certain amounts of nanoporous skeleton metal hybrid catalysts and cocatalysts, a reaction liquid is subjected to membrane separation, the catalysts can be repeatedly used for more than 7 times, and distilled to obtain nitroalkane products, the purity of the products is not less than 99%, and the yield of the products is not less than 95%. Furthermore, the green synthesis method for preparing nitroalkanes by the oxime oxidation disclosed by the invention is a green synthesis method of nitroalkanes, and suitable for large-scale industrialized production.
Method for preparing 2-nitropropane
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Paragraph 0016-0017, (2017/06/20)
The invention discloses a method for preparing 2-nitropropane, and relates to the technical field of organic compound synthesis. The method comprises the following steps: enabling acetone, ammonia gas or ammonia water, hydrogen peroxide, a solvent and a catalyst to contact, heating till the reaction temperature of 30-100 DEG C, and controlling the reaction pressure to 0.1-0.2MPa to react, thereby obtaining 2-nitropropane, wherein the catalyst is a TS-1 titanium silicalite molecular sieve; the solvent is water; the mole ratio of acetone to ammonia gas or ammonia water is 1:(1-3); the mole ratio of acetone to hydrogen peroxide is 1:(0.5-2); and the mass ratio of acetone to the catalyst is 1:(0.2-0.4). The method disclosed by the invention has the advantages that the conversion rate of acetone is high and the selectivity of 2-nitropropane is good; the method is simple in reaction process, gentle in reaction condition, environment-friendly and easy in industrial production; and development of environment-friendly chemicals is promoted.
A novel transition metal free [bis-(trifluoroacetoxy)iodo]benzene (PIFA) mediated oxidative ipso nitration of organoboronic acids
Chatterjee, Nachiketa,Bhatt, Divya,Goswami, Avijit
supporting information, p. 4828 - 4832 (2015/05/05)
A mild, convenient and transition metal free methodology for oxidative ipso nitration of diversely functionalized organoboronic acids, including heteroaryl- and alkylboronic acids, has been developed at ambient temperature using a combination of [bis-(trifluoroacetoxy)]iodobenzene (PIFA) - N-bromosuccinimide (NBS) and sodium nitrite as the nitro source. It is anticipated that the reaction proceeds through in situ generation of NO2 and O-centred organoboronic acid radicals followed by the formation of an O-N bond via combination of the said radicals. Finally transfer of the NO2 group to the aryl moiety occurs through 1,3-aryl migration to provide the nitroarenes.
Lewis acidic strength controlled highly selective synthesis of oxime via liquid-phase ammoximation over titanosilicates
Zhuo, Zuoxi,Wu, Lizhi,Wang, Lei,Ding, Yichun,Zhang, Xiaoqian,Liu, Yueming,He, Mingyuan
, p. 55685 - 55688 (2015/02/19)
The Lewis acidity of titanosilicates determines the selectivity of the oxime in ammoximation. Higher Lewis acidic strength of Ti active sites could promote free H2O2 to participate in the highly efficient formation of NH2OH by lowering the reaction activation energy for the formation of Ti-OOH species, and thus fundamentally suppress the side reactions of deep oxidation.
Process For Nitroalkane Recovery By Aqueous Phase Recycle To Nitration Reactor
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Page/Page column 5, (2011/05/03)
Disclosed are a process and an apparatus for synthesizing nitroalkanes by reaction of a hydrocarbon feedstock with aqueous nitric acid. Energy and capital costs may be reduced by recycling a majority of the aqueous phase back to the reactor.
PROCESS FOR THE MANUFACTURE OF NITRATED HYDROCARBONS
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Page/Page column 4-5, (2011/05/03)
Provided is a process for making nitrated hydrocarbons by reacting aqueous nitric acid with a hydrocarbon feedstock and a carboxylic acid under specific reaction conditions.
