Abstract: A synthetic process for the preparation of amino acid esters such as methylphenidate and analogs thereof is disclosed. The process involves reacting an amino acid such as ?-phenyl-?-(2-piperidinyl)acetic acid or an analog thereof with an alcohol such as methanol in the presence of an acid and a water sequestrant such as trimethyl orthoacetate. In some embodiments, the water sequestrant is added to the reaction mixture after an initial period of esterification and then the reaction is allowed to continue. The ?-phenyl-?-(2-piperidinyl)acetic acid methyl ester or analog thereof is then isolated from the reaction mixture. In one variation of the process, the supernatant liquid may be recycled in subsequent runs to increase yield and product purity.

Abstract: A synthetic process for the preparation of amino acid esters such as methylphenidate and analogs thereof is disclosed. The process involves reacting an amino acid such as ?-phenyl-?-(2-piperidinyl)acetic acid or an analog thereof with an alcohol such as methanol in the presence of an acid and a water sequestrant such as trimethyl orthoacetate. In some embodiments, the water sequestrant is added to the reaction mixture after an initial period of esterification and then the reaction is allowed to continue. The ?-phenyl-?-(2-piperidinyl)acetic acid methyl ester or analog thereof is then isolated from the reaction mixture. In one variation of the process, the supernatant liquid may be recycled in subsequent runs to increase yield and product purity.

Abstract: A method for controlling the direct process to vary the concentrations of trialkylhalosilanes and alkyltrihalosilanes in the product. The method comprises contacting an alkyl chloride with silicon metalloid in the presence of a catalytic amount of a catalyst comprising 0.5 to 10 weight percent copper, 5 to 200 ppm tin, 25 to 2,500 ppm phosphorous, and greater than zero to less than 50 ppm zinc, where the concentration of each of the catalyst components is based on the weight of the silicon, at a temperature within a range of about 250.degree. C. to 400.degree. C. The present inventors have found that by controlling the zinc concentration the concentrations of trialkylhalosilanes and alkyltrihalosilanes in the product can be varied.

Abstract: The present invention is a method for analyzing silicon for nonmetallic contaminants. The method comprises: (A) forming an alloy comprising silicon and a metal which promotes separation of nonmetallic contaminants present in the alloy, (B) separating the nonmetallic contaminants from the alloy, and (C) analyzing the separated nonmetallic contaminants for chemical content. The present invention is particularly useful for analyzing metallurgical grade silicon intended for use in the direct process for the production of organohalosilanes for the presence of oxides and carbides of calcium, aluminum, and silicon.

Abstract: The present invention is an improvement of the Direct Process for the manufacture of alkylhalosilanes by the contact of powdered metallurgical grade silicon with an alkyl halide in the presence of a copper catalyst. The improvement reduces lot-to-lot variations in silicon conversion to desired dialkyldihalosilanes. The improvement comprises alloying 0.01 to nine weight percent copper with the silicon to be used in the process and separating slag. In a preferred embodiment of the present process, silicon-copper alloy is pulverized to a powder and mixed with additional copper and other catalysts to form a contact mass reactive with alkylhalides.

Abstract: The described invention is a process for preparing silanes from the reaction of solid silicon monoxide with aromatic halides. The solid silicon monoxide is reacted with the aromatic halide in the presence of a catalyst which can increase the conversion of silicon monoxide to silanes, and partially select for arylsilane products. The process may employ an activation step in which the solid silicon monoxide is activated by heating in an inert atmosphere. Activation of the solid silicon monoxide can increase silicon conversion and increase selectivity for arylsilane products.

Abstract: The present invention is processes for preparing silanes from the reaction of silicon monoxide with hydrogen halides. In a first embodiment of the instant invention, silicon monoxide is reacted with a hydrogen halide to produce silanes and halosilanes. In a second embodiment of the instant invention, the silicon monoxide is activated by heating in an inert atmosphere prior to contact with the hydrogen halide. In a third embodiment of the instant invention, a catalyst is employed which enhances conversion of silicon monoxide to silanes and modifies process selectivity for silane products. The catalyzed process can be run with activated or non-activated silicon monoxide.

Abstract: The present invention is a process for preparing silanes from the reaction of solid silicon monoxide with organic halides. The solid silicon monoxide is reacted with the organic halide in the presence of a catalyst which can increase the conversion of silicon monoxide to silanes and partially select for the type of silanes produced. The process may employ an activation step in which the solid silicon monoxide is activated by heating in an inert atmosphere. Activation of the silicon monoxide can increase silicon conversion and alter the type of silanes produced.

Abstract: A method for rendering an aluminum electrowinning cell component fabricated from an aluminum nonwettable material wettable by molten aluminum, and therefore utilizable within the cell. Under the method, the component is coated with titanium and boron, and while the component is immersed in molten aluminum within the cell, the molten aluminum is maintained near saturation with boron and titanium.

Abstract: A method and apparatus for making a drained aluminum electrowinning cathode dimensionally stable. A thin, 1/2 to 10 millimeter coating of substantially stagnant molten aluminum is maintained upon the cathode surface by an openly porous sheath or membrane closely conforming to contours of the electrowinning cathode. The sheath or membrane is made from a material substantially resistant to corrosives present in the aluminum electrowinning; it may be only slightly aluminum wettable, but should be relatively electrically nonconductive.