Bi2S3 and Sb2S3 nanorods were synthesized from single-source precursors M(S2CNEt2)(3) (M = Bi, Sb) via a hydrothermal treatment. The X-ray powder diffraction patterns show that both of the products belong to the orthorhombic M2S3 phase. Energy-dispersive X-ray analysis shows the products are phase pure. Transmission electron microscopic (TEM) and scanning electron microscopy (SEM) studies reveal the rodlike appearance of either Bi2S3 or Sb2S3 with a diameter in the range of 50-400 nm and a length in the range of 1-7 mum. The experimental results show that the nanorods can be prepared in protic solvent under experimental conditions (at 115-170 degreesC for 10 h). A possible mechanism is discussed.