N-(Hydroxymethyl)thioamides are readily available compounds that are widely used in the synthesis of nitrogen- and sulfur–containing heterocycles such as 1,3-thiazines, 1,2,4-dithiazoles, 1,3,5-oxathiazines, 1,3,5-thiadiazines, thiazolidines, and others. In addition to its use in fine organic synthesis, N-(hydroxymethyl)thioamides are also used for other purposes. For example, some representatives of this class act as bidentate ligands to create selective sorbents for heavy metal ions such as Cu(II), Cd(II) and Hg(II). These compounds are intermediates in the synthesis of a number of biologically active substances. At the same time, a limited number of methods for obtaining compounds of this type are presented in the literature, and the variability of structures is not high enough. Thus, N-(hydroxyalkyl)thioamides belong to a promising group of compounds, and the development of methods for the synthesis of such compounds can be considered an important problem. Cyanothioacetamide readily reacts with aromatic aldehydes in an aqueous alcohol medium in the presence of triethylamine as a catalyst to form arylmethylenzyanothioacetamides (3-aryl-2-cyanothioacrylamides). The latter reacted with HCHO to give N-(hydroxymethyl) derivatives. In this paper, a method for preparation of new derivatives of N-(hydroxyalkyl) thioacrylamides was proposed. The synthetic details and spectral data are discussed. The biological effects as herbicide 2,4-D safeners is also discussed.