An improved synthesis of tetramethylammonium azide, N(Me)(4)N-+(3)-, is pre
sented. It involves a neutralization of tetramethylammonium hydroxide with
sulfuric acid, followed by a metathetical reaction with sodium azide in met
hanol. Tetramethylammonium azide is then separated from the less soluble Na
2SO4 via filtration. This method provides a convenient access to tetramethy
lammonium azide. It is therefore more usable in a typical academic laborato
ry setting than previously reported syntheses.