Abstract: A process for preparing 2,6-dimethylphenylisothiocyanate comprises the steps of dissolving 2,6-dimethylaniline in carbon disulfide and ammonium hydroxide to form a dithiocarbamate salt. The salt is reacted with ethyl chloroformate to form 2,6-dimethylphenylisothiocyanate, which may thereafter be reacted with 3-amino-1-propanol and subsequently cyclized, by treating with hydrochloric acid, to form xylazine.