Non-hydrolytic sol-gel reactions provide a low temperature solution based synthetic approach to solid-state materials. In this paper, reactions between molybdenum chloride and hexamethyldisilthiane in chloroform were explored, which gave access to both MoS 2 and Mo 2 S 3 after heat treatment of as-recovered amorphous samples to 600 to 1000 C. Interesting morphologies were obtained for MoS 2 , ranging from fused spherical particles to well-defined nanoplatelets and nanoflakes. Both 2H-and 3R-MoS 2 were observed, which formed thin hexagonal and triangular platelets, respectively. The platelets exhibited thicknesses of 10 to 30 nm, which corresponds to 15 to 50 MoS 2 layers. No attempts to prevent agglomeration were made, however, well separated platelets were observed for many samples. Heating at 1000 C led to formation of Mo 2 S 3 for samples that showed well-defined MoS 2 at lower temperatures, while less crystalline samples had a tendency to retain the MoS 2 structure.