A new method for the synthesis of the tit1e compounds 6 is described in this paper. Compounds 6 were obtained by an one-pot reaction process from β-dione and its analogues, 2-bromoethanol and carbon disulfide with potassium carbonate as the base. The possible mechanism is discussed. In this mechanism, a monoanion intermediate 3 is proposed, it reacts with 2-bromoethanol by a sequential nucleophilic and electrophilic reaction process to build the key intermediate 5. 6 is formed by the elimination of hydrosulfide from 5.