1. Acetyl thioctic acid has been prepared chemically and i t s chromatographic and acetylating behavior i s described. 2. A C{sup 14} -containing substance has been found in Scenedesmus, photosynthesizing in the presence of a-C{sup 14}-pyruvate, which has properties suggesting that it i s acetyl thioctic acid. 3 . A C{sup 14}-containing substance has been found in Aerobacter aerogenes, metabolizing a-C{sup 14}-pyruvate, which shows the properties of a labile conjugate of thioctic acid with some relatively polar groups. 4. Acetyl thioctic acid i s formed in vitro when light acts on a solution of thioctic acid and pyruvate.