Trifluorothiolacetic acid (CFaCOSH) was first prepared by Sheppard and Muetterties3 by allowing (CFa-CO), O and HzS to react together at 200" in 45% yield. The chemistry of CF, COSH has received very little attention, and only one paper3 has appeared in the literature. The presence of the SH group offered a way to prepare new sulfenyl halides and sulfides which contained the highly reactive trifluoroacetyl group.