Abstract: A process for the preparation of bromostyrenes which comprises aqueous alcoholic alkali dehydrohalogenation of a 1-haloethyl bromobenzene, a 2-haloethyl bromobenzene, or a 1-methyl-2-haloethyl brominated benzene in the presence of a phase transfer catalyst at a temperature of between about 0.degree. C. and about 150.degree. C. The bromostyrenes have the particular utility as a comonomer for the preparation of a co-polymer exhibiting a flame retardancy. Both bromostyrenes and brominated alpha-methyl styrenes are formed.
Abstract: Alkali metal aluminum tetraalkyls can alkylate tetraalkyl silicates and alkyltrialkoxysilanes, Si(OR).sub.4 and RSi(OR).sub.3, respectively. The product in each case is predominately the dialkylate. With tetraalkyl silicates, both of the alkyl groups bonded to silicon in the dialkylate product are derived from the metal tetraalkyl. With alkyltrialkoxysilanes, the silicon atom in the dialkylate product is (a) bonded to one alkyl group detained from the metal tetraalkyl, and (b) is also bonded to an alkyl group--that was bonded to silicon--in the silicon-containing starting material. Thus, the alkyl groups in the dialkylate product that are bonded to silicon can be alike or different. The dialkyldialkoxysilane products produced by this invention can be reduced to the corresponding silanes; e.g., R.sub.2 SiH.sub.2, by using an alkyl aluminum tetrahydride as the reducing agent. The dialkyldialkoxysilanes as well as the dialkylsilanes produced are useful as chemical intermediates.
Abstract: 1-[2,5-Bis(2,2,2-trifluoroethoxy)phenyl]ethanone is chlorinated to 1-[2,5-bis(2,2,2-trifluoroethoxy)phenyl]-2,2-dichloroethanone and, if desired, to 1-[2,5-bis(2,2,2-trifluoroethoxy)phenyl]-2,2,2-trichloroethanone in a solvent mixture of about 0.5-35 parts by volume of 1,2-dichloroethane and one part by volume of acetic acid. The products can then be converted to flecainide. In a preferred embodiment of the invention, the starting material is a crude, wet material that is prepared with a minimum of solids handling.
Abstract: A method of folding large sheets of tubular plastic film or slit tubular plastic film wherein the longitudinal edges of the plastic film are folded back over a surface of the film about 180.degree. to an imaginary longitudinal line drawn substantially through the center of a surface of the film and then forming the so-folded sheet into a roll and a roll of greenhouse film folded in the foregoing manner.
Abstract: An olefin, especially an activated olefin, is telomerized by reaction with an arylamine, such as an aniline, in the presence of an alkyl nitrite, a copper catalyst, and a catalytic amount of water and/or acid and in the absence of more than about 0.5 volume part of inert solvent per volume part of olefin.
Abstract: Silane and monoalkylsilanes can be alkylated using an alkali metal aluminate, MAlR.sub.4, wherein M is Li, Na, or K and each R is a straight chain, alkyl radical solely composed of carbon and hydrogen containing from about 4 to about 18 carbon atoms. The aluminate can be used as a reactant, optionally in the presence of a straight chain alpha-olefin corresponding to the alkyl group in the aluminate. Alternatively, the aluminate can be used as a catalyst for the reaction of the olefin and the silane reactant, in which case from about 5 to about 10 mole percent of the aluminate (based on the silane reactant) is employed. The catalytic reaction is promoted by a smaller amount of a lithium salt such as lithium chloride. Both embodiments are conducted at somewhat elevated temperatures, approximately 160.degree.-210.degree. C., and at autogenous pressures, using reaction times of 8-20 hours.The products are useful as functional fluids or as intermediates.
September 18, 1986
Date of Patent:
June 2, 1987
Arcelio J. Malcolm, Charles R. Everly, Gunner E. Nelson
Abstract: Saturated hydrocarbon is transformed catalytically into olefinic hydrocarbon of corresponding skeletal configuration by reacting the saturated hydrocarbon with a suitable alkene cyclopentadienyl or alkene arene transition metal molecular complex, such as bis(ethylene)pentamethylcyclopentadienyliridium, in the presence of free alkene as hydrogen acceptor. The reaction may be performed photochemically under irradiation with ultraviolet light or it may be performed thermolytically under application of heat. The catalyst may be charged to the reaction as a preformed alkene cyclopentadienyl or alkene arene transition metal molecular complex or the catalyst may be formed in situ in the reaction mixture via displacement of ligand from a suitable transition metal complex containing the displaceable ligand, such as dicarbonylpentamethylcyclopentadienyliridium or cyclooctadienepentamethylcyclopentadienyliridium.
Abstract: (Hydrocarbylthio)aromatic amines are prepared by reacting an aromatic monoamine, such as an aminobenzene, with a hydrocarbyl disulfide, such as an alkyl disulfide, in the presence of hydrogen iodide, ammonium iodide, or cuprous iodide.
Abstract: (Hydrocarbylthio)aromatic polyamines are prepared by reacting an aromatic polyamine, such as a diaminobenzene, with a hydrocarbyl disulfide, such as an alkyl disulfide, in the presence of an iodide or bromide of a metal other than an alkali metal as a catalyst.
Abstract: A reactor apparatus (10) adapted for continuously producing molten, solar grade purity elemental silicon by thermal reaction of a suitable precursor gas, such as silane (SiH.sub.4), is disclosed. The reactor apparatus (10) includes an elongated reactor body (32) having graphite or carbon walls which are heated to a temperature exceeding the melting temperature of silicon. The precursor gas enters the reactor body (32) through an efficiently cooled inlet tube assembly (22) and a relatively thin carbon or graphite septum (44). The septum (44), being in contact on one side with the cooled inlet (22) and the heated interior of the reactor (32) on the other side, provides a sharp temperature gradient for the precursor gas entering the reactor (32) and renders the operation of the inlet tube assembly (22) substantially free of clogging. The precursor gas flows in the reactor (32) in a substantially smooth, substantially axial manner.
Abstract: Oxazepinones and thiazepinones correspoding to the formula: ##STR1## are prepared by mixing an alkali metal salt corresponding to the formula ##STR2## with oxalyl chloride or bromide in an inert solvent and heating to effect halogenation and fusion, A in the formulas representing a substituted or unsubstituted benzene, naphthalene, or pyridine ring bearing up to two Y substituents; E being oxygen or sulfur; R being an alkyl, cycloalkyl, or phenalkyl group or a substituted phenalkyl group bearing up to two ar-Y substituents; X being chloro or bromo; M being an alkali metal; n being one or two; and Y being a substituent selected from alkyl, alkoxy, trifluorimethyl, nitro, and halo. The products are useful as pharmaceutical intermediates.
Abstract: A process for producing complexes of alane and tertiary amines. Sodium aluminum tetrahydride is reacted with sodium aluminum tetrachloride in the presence of a tertiary amine in an aromatic hydrocarbon reaction medium that is not a solvent for either of the reactants. The tertiary amine alane reaction products are typically soluble in the hydrocarbon reaction medium and readily recoverable.
Abstract: Polymer-grade cyclic phosphonitrilic halide trimer can be obtained by (i) reacting ammonium halide with phosphorus pentahalide in an inert solvent containing pyridine, substituted pyridines or mixtures thereof or hydrogen halide complexes thereof, (ii) washing the solvent phase with an aqueous alkali metal hydroxide and (iii) crystallizing cyclic trimer and/or distilling the cyclic trimer to obtain polymer-grade trimer.
April 21, 1986
Date of Patent:
May 5, 1987
Joseph B. Tedder, Jr., J. Robert Adams, Jr.
Abstract: An organic carbonyl compound is thiated to the corresponding thiono compound by reacting it with phosphorus pentasulfide in the presence of an alkali metal bicarbonate and a hydrocarbon diluent. In preferred embodiments of the invention, the carbonyl compound is an amide, especially an aromatic amide, and the diluent is an inert hydrocarbon having a boiling point in the range of about 50.degree.-150.degree. C.
Abstract: Polyetheroxy-substituted polyphosphazenes having reduced mono and polyetheroxy alkanol, alkali metal and halide contaminants that are suitable for use in making solid electrolytes are made by dissolving the impure polyphosphazene in an inert solvent (e.g. tetrahydrofuran) and mixing this solution with a cycloalkane (e.g. cyclohexane) to precipitate the polyetheroxy-substituted polyphosphazene with reduced etheroxy alkanol content. This can be dissolved in water and contacted with an anion exchange material to remove residual halide anions. The purified polyetheroxy-substituted polyphosphazene is then recovered by distilling off the water.
Abstract: Water-soluble polymers of monoallylamine are employed to coalesce suspended particulate matter in aqueous dispersions. This enables rapid and efficient separation between coalesced solids and the aqueous medium by any of a variety of conventional physical techniques such as settling and decantation, filtration, centrifugation, and the like.
Abstract: A process for purifying crude brominated aromatic compounds such as decabromodiphenyl oxide containing impurities. The crude brominated aromatic compound undergoes a single processing step of grinding in the presence of heated air. The temperature is sufficient to effect substantial removal of impurities and yet remains below the melting point of the brominated aromatic compound.