Amines react with DMF-NO2 adduct under nonaqueous condition to give solid aryl diazonium nitrate in high purity and excellent yield.
Zhang, Z.; Liu, X.; Zhang, Q., Organic Preparations and Procedures International, 2001, vol. 33, # 3, p. 305 - 310
作者:Zhang, Z.、Liu, X.、Zhang, Q.、Zhang, S.、Huang, T.
DOI:——
日期:——
Abfallfreie Gas/Festkörper-Diazotierung mit Stickstoffdioxid und quantitative Triazensynthese ohne Flüssigphase
作者:Gerd Kaupp、Andreas Herrmann
DOI:10.1002/prac.19973390145
日期:——
Solid diazonium nitrates (2a-j) are quantitatively obtained by reaction of crystalline anilines (1a-j) with gaseous nitrogen dioxide. Solid diazonium salts react quantitatively with dimethylamine to give the triazenes (4a-j). Wastes that are typical for the previous syntheses of these compounds in solution are avoided. Atomic force microscopic (AFM) investigations indicate long-range molecular movements due to phase rebuilding. The features thus formed are related to the known crystal structures of the starting anilines. The diazotations run to completion, because, after accumulation of product molecules, phase transformation to give the product lattices leads to crystal disintegration and thus to formation of fresh surface over and over.