Abstract:
p-Nitrophenolic compounds, e.g., p-nitrophenol itself, are selectively prepared by (a) reacting a phenolic compound with a nitrosating agent in the presence of sulfuric acid, the concentration of which H.sub.2 SO.sub.4 being at least 60%, (b) oxidizing the p-nitrosophenolic compound thus formed with nitric acid, the concentration of sulfuric acid in the medium of reaction, upon completion of oxidation, being no greater than 80%, and (c) separating the p-nitrophenolic compound which thus precipitates.
Abstract translation:通过(a)在硫酸存在下使酚类化合物与亚硝化剂反应,其中H 2 SO 4的浓度为至少60%,(b)将硝基酚类化合物氧化为 由硝酸形成的对亚硝基苯酚化合物,氧化后的反应介质中的硫酸浓度不大于80%,(c)分离因此析出的对硝基酚化合物。
Abstract:
A continuous process for the preparation of isomeric mixtures of dinitrotoluene by a single stage nitration of toluene under adiabatic conditions. The reaction enthalpy is used for the removal by distillation of the water of reaction formed during nitration. In this process, toluene is reacted with a nitrating acid having from about 80 to about 100% by weight of an inorganic component having a specified composition and from about 0 to about 20% by weight of an organic component having a specified composition.
Abstract:
Improved process for preparing dinitrotoluene by reacting toluene with concentrated nitric acid. The process reacts toluene with a large excess of concentrated nitric acid, in the presence of a select hydrated nitrate salt which is effective in minimizing explosive hazards, to produce a product which has substantially reduced by-product content.
Abstract:
Process for preparing dinitrotoluene by reacting toluene with concentrated nitric acid. The process reacts toluene with a large excess of concentrated nitric acid at selected conditions to produce a product which has substantially reduced by-product content.
Abstract:
A method of preparing 2-bromo-4,6-dinitromesitylene having only small amounts of impurities, by first mixing fuming sulfuric acid with bromomesitylene, and then adding concentrated nitric acid.
Abstract:
A regioselective nitration process for diphenyl compounds which can be carried out at about ambient temperature in which each ring of the diphenyl compound is selectively nitrated in the para position to form the corresponding di(4-nitrophenyl) compound. Such compounds as diphenyl carbonate, 2,2-diphenylpropane, 2,2-diphenylhexafluoropropane, diphenyl sulfide, diphenyl ketone, diphenyl sulfone, and the like can be converted to an isomeric mixture containing an enhanced amount of the corresponding di(4-nitrophenyl) compound, which mixture may be reduced or purified and reduced to the di(4-aminophenyl) analogues for use in the manufacture of polyamides, polyimides, and polyamide-imides.
Abstract:
Preparation of 1,3,5-triamino-2,4,6-trinitrobenzene (TATB) from 3,5-dichloroanisole. Nitration of 3,5-dichloroanisole under relatively mild conditions gave 3,5-dichloro-2,4,6-trinitroanisole in high yield and purity. Ammonolysis of this latter compound gave the desired TATB. Another route to TATB was through the treatment of the 3,5-dichloro-2,4,6-trinitroanisole with thionyl chloride and dimethylformamide to yield 1,3,5-trichloro-2,4,6-trinitrobenzene. Ammonolysis of this product produced TATB.
Abstract:
An improved nitric acid only nitration process wherein the improvement comprises adding an effective amount of a nitration promoting acid anhydride to the reaction mixture to enhance the rate of nitration.
Abstract:
Infrared laser-induced production of nitrated products is achieved by irradiating compounds selected from propane, n-butane, isobutane, n-pentane, and cyclopropane in the gas phase while in a stainless steel cell 5.times.5.times.10 cm equipped with zinc selenide windows to admit the infrared laser radiation in the range of 10.4 or 9.4 micrometers provided by a continuous wave CO.sub.2 laser. KC1 windows on the short path are to monitor infrared spectra of reactants and products. Nitrogen dioxide or nitric acid is present as the second reactant and the nitrating agent. The infrared laser-induced method far exceeds the yield of nitrated products found in the argon-ion laser-induced nitration of isobutane reported in the literature. Applicants' method at least equals the yield from thermally activated systems with a minimum formation of undesirable side products. A representative sample, 220 torr of gaseous butane, and 20 torr NO.sub.2 is irradiated in one experiment for 30 seconds with 75 W/cm.sup.2 at a frequency of 956 cm.sup.-1. About 40% of the NO.sup.2 is converted to nitrocompounds. Identified as nitro-products are nitromethane, nitroethane, 1-nitropropane, 1-nitrobutane and 2-nitrobutane. More than 60% of the nitro-products are in the long chain forms, 1-nitrobutane and 2-nitrobutane. Pressure of the NO.sub.2 reactant range from about 20 to 30 torr while the hydrocarbon reactant pressure range from about 200 to about 500 torr. Irradiation times ranges from about 30 to about 60 seconds. Laser powers range from 75 watts/cm.sup.2 to about 82 watts/cm.sup.2.
Abstract translation:通过在气相中照射选自丙烷,正丁烷,异丁烷,正戊烷和环丙烷的化合物来实现硝化产物的红外激光诱导产生,同时在5×5×10cm的装有硒化锌窗口的不锈钢电池中容纳红外线 激光辐射范围为10.4或9.4微米,由连续波CO2激光器提供。 短路上的KC1窗口是监测反应物和产物的红外光谱。 存在二氧化氮或硝酸作为第二反应物和硝化剂。 红外激光诱导的方法远远超过文献报道的氩离子激光诱导的异丁烷硝化中发现的硝化产物的产率。 申请人的方法至少等于热活化系统的产量,最少形成不希望的副产品。 一个代表性的样品,220托的气态丁烷和20托的NO 2在一个实验中以75W / cm 2的频率在956cm -1处照射30秒。 约40%的NO2转化为硝基化合物。 硝基甲烷,硝基乙烷,1-硝基丙烷,1-硝基丁烷,2-硝基丁烷等。 硝基产物超过60%是长链形式,1-硝基丁烷和2-硝基丁烷。 NO 2反应物的压力范围为约20至30托,而烃反应物压力范围为约200至约500托。 照射时间范围为约30至约60秒。 激光功率范围为75瓦特/平方厘米至约82瓦特/平方厘米。
Abstract:
The present invention relates to improvements in processes of preparing dinitrated .[.aromatic compounds, particularly dinitrated aniline and dinitrated substituted aniline compounds, employing relatively dilute and then more concentrated nitric acid as the nitrating agent.]. .Iadd.aniline and substituted phenol compounds in a two-step process, employing, in the first or mononitration step the spent nitric acid from the second of dinitration step. .Iaddend.