S-Alkyl thiocarbamates are commercially available and widely used for their herbicidal properties. Despite the numerous methods for synthesizing these compounds, most employ toxic reagents that are harmful to the environment. Within we report a novel efficient one-pot process for the formation of thiobencarb employing readily available reagents. This method makes use of a trichloroacetyl chloride adduct and requires no complex starting materials. Furthermore, this process is efficient, proceeds in high yields, and utilizes several recyclable reagents.