Aerojet-general Corporation

James C Barnard

Thomas G Archibald

Der-Shing Huang

Robert Earl Olsen

Renato R Rindone

Harlan Frederick Reese

Donald M Kunkle

George D Homer

Mark H Pratton

Ernest W Leachty

Bennie L Benning

4-Sulfonamidophenyl hydrazines are prepared by reaction between the hydrazine, optionally substituted, and the corresponding 4-substituted benzenesulfonamides, where the 4-substitution is an appropriate leaving group, in the presence of water and the absence of dimethyl sulfoxide as a solvent. The result is a product of unusually high purity.

Process for 4-sulfonamidolphenyl hydrazines

Diazomethane is produced in a continuous process with little or no explosion hazard, by dissolving an N-methyl-N-nitroso amine in a mixture of a water-miscible organic solvent that dissolves the N-methyl-N-nitroso amine and a water-immiscible organic solvent that dissolves diazomethane, and combining a stream of this solution with a stream of an aqueous inorganic base, allowing the aqueous and organic phases to settle after a suitable residence time, and phase separating the phases, all on a continuous basis. When using N-methyl-N-nitrosourea as the amine, the diazomethane process is preceded by a continuous nitrosation process involving combining aqueous solutions of methyl urea and a nitrite salt with an organic solution of a mineral or organic acid, the solvent in the organic solution being a mixture of the two organic solvents referred to above, allowing the aqueous and organic phases to settle after a suitable residence time, and phase separating the phases, all on a continuous basis. The resulting organic phase is continuously fed to the diazomethane stages described above.

Continuous process for diazomethane from an n-methyl-n-nitrosoamine and

Alkyl-substituted polyarenes of the formula ##STR1## in which R is alkyl and Ar.sub.res is an aryl residue, are prepared from aryl ketones by reaction of the latter with 1-cyclohexenyloxytrimethylsilane in the presence of a Friedel-Crafts catalyst. When R is methyl and Ar.sub.res is a naphthyl residue, the reaction serves as a step in a reaction scheme leading to crisnatol mesylate, a pharmaceutical useful in the treatment of brain cancer.

Polyarenes from aryl ketones with application to synthesis of crisnatol

Diazomethane is prepared in a batch process on a scale of at least 50 gram-moles per batch, from an N-methyl-N-nitroso amine in an organic solvent and an inorganic base in an aqueous solution by the use of a phase transfer catalyst and by controlling the choice of solvent, reagent concentrations, addition rate and reaction temperature to cause codistillation of the product and the organic solvent in such a manner that the concentration of diazomethane in both liquid and vapor phases are controlled within limits that will prevent detonation of the diazomethane.

Large scale batch process for diazomethane

Solid energetic compositions such as rocket motor grains are desensitized and converted to a form suitable for incineration by size reducing the solids, combining them with water to form a slurry, and adding shredded paper or similar cellulosic material in an amount sufficient to absorb most if not all of the water. The result is a composition which is non-detonable, and yet capable of incineration in a clean manner to produce useful by-products.

Desensitization of cured energetic compositions in aqueous media

A method of making ethylenediamine dinitrate comprising:

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Shingle Springs, CA, United States of America

James C Barnard