Abstract:
High purity 4,6-dinitro-1,3-benzenediol is prepared by (a) contacting a 1,2,3-trihalobenzene with a nitrating agent and an acid under reaction conditions such that a 1,2,3-trihalo-4,6-dinitrobenzene is produced, (b) contacting the 1,2,3-trihalo-4,6-dinitrobenzene prepared in (a) with an alkanol and a base under reaction conditions such that a 4,6-dinitro-2-halo-1,3-benzenediol is produced, and (c) contacting the 4,6-dinitro-2-halo-1,3-benzenediol prepared in (b) with a hydrogenating agent in the presence of a solvent and a catalyst under reaction conditions such that a 4,6-diamino-1,3-benzenediol is produced. This 4,6-diamino-1,3-benzenediol is useful in the preparation of high molecular weight polybenzoxazoles.
Abstract:
Catalysts comprising the adduct of a Group 4b-Group 3b metal oxide composition represented by the empirical formula:(M.sup.1.sub.a M.sup.2.sub.b O.sub.c).sub.x (NO.sub.2).sub.ywherein M.sup.1 is at least one element selected from Group 4b of the Periodic Table of the Elements, M.sup.2 is at least one element selected from Group 3b of the Periodic Table of the Elements, a is 1, b is 0.05 to 20, c is a number taken to satisfy the average valences of M.sup.1 and M.sup.2 in the oxidation states in which they exist in the composition, x is 1, and y is 0 to c, and a catalytically effective amount of sulfur trioxide are useful to catalyze the nitration of aromatic compounds in the vapor phase to produce nitroaromatic compounds. The catalysts are particularly effective to catalyze the vapor phase nitration of chlorobenzene and are characterized in such reaction by providing a para/ortho isomer distribution ratio of at least about 2/1.
Abstract:
Substituted phenols are nitrated by contacting same with a 10 to 70% by weight concentrated aqueous solution of nitric acid. The subject nitration process is well adopted for the preparation, e.g., of 2,6-dichloro-4-nitrophenol, a valuable intermediate in the production of various agrochemicals/pharmaceuticals.
Abstract:
Aromatic compounds are nitrated in the vapor phase via a process comprising contacting the aromatic compounds with a nitrating agent in the presence of a nitration promoting catalyst comprising the adduct of a Group 4b-Group 3b metal oxide composition represented by the empirical formula:(M.sup.1.sub.a M.sup.2.sub.b O.sub.c).sub.x (NO.sub.2).sub.ywherein M.sup.1 is at least one element selected from Group 4b of the Periodic Table of the Elements, M.sup.2 is at least one element selected from Group 3b of the Periodic Table of the Elements, a is 1, b is 0 to 20, c is a number taken to satisfy the average valences of M.sup.1 and M.sup.2 in the oxidation states in which they exist in the composition, x is 1, and y is 0 to c, and a catalytically effective amount of sulfur trioxide. Such catalysts are particularly effective to catalyze the vapor phase nitration of chlorobenzene and are characterized in such reaction by providing a para/ortho isomer distribution ratio of at least about 2/1.
Abstract:
Dinitro alkyl phenols are produced free of tar when the precursor orthoalkylphenol is contacted with a molecular sieve prior to sulfonation, nitration, and air drying. The dinitro alkylphenols produced are free of tars or similar resins and avoid processing problems that are shown in impure prior art products.
Abstract:
A reactor for nitration of saturated hydrocarbons having less than five con atoms, alone or in admixture, in the gaseous phase under pressure is made up of a reaction enclosure, in which a tube or pipe bank is in contact with a heated fluid of high heat-exchange capacity. The inside perimeter of the tubes does not exceed 800 mm, and if circular not in excess of 250 mm, and the ratio of the surface of the tube bank, in contact with the reaction medium, to the volume of the reaction enclosure is 1:1 to 3:1.The reactor apparatus further includes a mechanical means to uniformly distribute the delivery of reaction medium gases to the various tubes of the bank so that the load difference between the most loaded tube and that of the least loaded tube is equal to 10% at the most.The reactor also includes a tube bank injector which feeds the tube bank to assure homogeneous mixing of all the reaction fluids in the tube bank.
Abstract:
Dinitrotoluene, which is produced by mixed acid nitration of toluene, is purified in a way which produces a product suitable for conversion to toluene diamine and a less environmentally objectionable by-product stream. The process involves contacting a crude dinitrotoluene stream containing by-product nitrophenolic materials with an alkaline material and monitoring the pH such that dinitroorthocresol by-product is maintained in the organic phase while the trinitroorthocresol by-products are converted to water-soluble materials and removed with an aqueous phase.
Abstract:
A streamline flow of aqueous cobalt (II) sulphate solution passes through a platinum tube which, as an anode, electrolyses the solution to cobalt (III). The flow, with a high surface concentration of nascent cobalt (III), falls into a volume of 1-methylnaphthalene in an organic solvent, and is recovered from underneath for recycling to the platinum tube anode.The cobalt (III) reacts with the 1-methylnaphthalene to form 1-naphthaldehyde. Other oxidations of organic reactants using nascent high-oxidation-state aqueous metal ions are also disclosed.
Abstract:
Diphenyl esters of the formula ##STR1## wherein R is hydrogen, carboxy, carboxylate salt or ester, formyl, cyano, alkyl, alkoxy, chloro, bromo, or N, N-dialkyl amino, are prepared by reacting a chloro-fluoro-benzotrifluoride with a nitro-phenoxide of the formula ##STR2## where R is defined above, and M is a cation of an alkali metal or an alkaline earth metal.
Abstract:
Aromatic hydrocarbons are nitrated by reacting the aromatic hydrocarbon in a nitrogen tetroxide-containing liquid reaction medium, in the presence of a beta-dicarbonyl compound having a "W" configuration with a carbonyl group at each apex of the "W", such as a metal acetylacetonate, preferably at a pressure and temperature sufficient to maintain the nitrogen tetroxide in the liquid state. Addition of an inert organic co-solvent to the liquid nitrogen tetroxide for the metal acetylacetonate promoted nitration of benzene essentially eliminates the production of dinitrobenzenes.