Tetrasulfur Tetranitride - Synthesis

Synthesis

S4N4 was first prepared in 1835 by W. Gregory, by the reaction of sulfur monochloride with ammonia.

Until recently, S4N4 was prepared by the reaction of ammonia with SCl2 in carbon tetrachloride followed by extraction into dioxane, producing sulfur and ammonium chloride as side-products:

24 SCl2 + 64 NH3 → 4 S4N4 + S8 + 48 NH4Cl

A related synthesis employs sulfur monochloride and NH4Cl instead:

4 NH4Cl + 6 S2Cl2 → S4N4 + 16 HCl + S8

A more recent synthesis entails the use of 2S as a precursor with pre-formed S–N bonds. 2S is prepared by the reaction of lithium bis(trimethylsilyl)amide and SCl2.

2 2NLi + SCl2 → 2S + 2 LiCl

The 2S reacts with the combination of SCl2 and SO2Cl2 to form S4N4, trimethylsilyl chloride, and sulfur dioxide:

2S + SCl2 + SO2Cl2 → S4N4 + 4 (CH3)3SiCl + SO2

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