Continuous process for diazomethane from an n-methyl-n-nitrosoam

Details Continuous process for diazomethane from an n-methyl-n-nitrosoam Continuous process for diazomethane from an n-methyl-n-nitrosoam

1997-11-13

1998-12-29

Higel, Floyd D.

Organic compounds -- part of the class 532-570 series

Organic compounds

Diazo or diazonium

534558, C07C24512, C07C24516

Patent

active

058544054

ABSTRACT:
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.

REFERENCES:
patent: 4197410 (1980-04-01), Sekiya et al.
patent: 5459243 (1995-10-01), Acevedo et al.
T.H. Black Aldrichimica Acta, (1983) 16(1): 3-10.

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