Azide synthesis in microstructured flow systems
MICHAEL WEBER, GOEKCEN YILMAZ, GREGOR WILLE*
*Corresponding author
Sigma-Aldrich Production GmbH, Industriestrasse 25, Buchs, 9471, Switzerland
Abstract
A process for synthesising organic azides starting fromthe corresponding amine is elaborated. It enables thesafe handling of a diazo intermediate (stage 1) andits subsequent treatment with sodium azide (stage 2).Accumulation of critical product was prevented byinjection of an organic solvent prior to stage 2 followed byinstant extraction. In order to minimise all risks arising frompotentially formed hydrazoic acid the aqueous productphase was continuously separated and inactivated. Thisenabled the daily manufacturing of 4.5-6 litre of azidesolution in 0.5 M standard concentration.
...