With the purpose to study the influence of thyroidectomy on the free amino acids and the related compounds the author performed the assay of 11 of these substances by ion exchange column chromatography, using the rat brains as the material. As the result it has been found that aspartic acid, glutamic acid, alanine, serine, N-acetylasparticacid, and glycerophosphoethanolamine, the substances that were decreased in the brains of hypophysectomized animals, have been maintained at the normal level on thyroidectomy.