Large scale batch process for diazomethane
AssigneeAerojet-General Corporation
InventorsThomas G. Archibald, Der-Shing Huang, Mark H. Pratton, James C. Barnard
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Abstract
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.
Claims19
A process for the production of diazomethane, comprising:
- (a) adding a solution of at least about 50 g-moles of an N-methyl-N-nitroso amine of the formula ##STR2## in which R is an electron-withdrawing radical, in an organic solvent that (ii) forms a separate phase when contacted with water and (i) has a boiling point less than about 40.degree. C., to a reaction vessel containing an aqueous solution of an excess of inorganic base relative to said N-methyl-N-nitroso amine and a phase transfer catalyst, while maintaining the contents of said reaction vessel at a temperature high enough to vaporize both said organic solvent and diazomethane thus formed, the rate of addition of said N-methyl-N-nitroso amine and the temperature of said reaction vessel maintained such that the diazomethane concentration in the liquid phase in said reaction vessel is maintained at 3 weight percent or less and the diazomethane concentration in the vapor phase thus formed is maintained at about 25 mole percent or less;
- and
- (b) condensing said vapor phase thus formed in (a) to form an organic liquid solution of diazomethane.
Dependencies are inferred from the claim text.