The reaction of o-acylthiophenacyl chloride 5a with onc equivalent ofsodium azide in aqueous acetone at-10~ $-5^{circ}C$ gave 2,9-dimethyl-6H,I3H-dibenzo[d,i][1,6]dithiecin-7,14-dione 7(10%),acyclic dimer 8(64%),and tri-mer 9 (8%). Dimer 8 and trimer 9 we re converted readily to 7 under the similar conditions at room temperature in yields of 72% and 53%,respectivel. Also, one pot synthesis of 7 (64%, 45%) from the reaction of 5a or 5b with two equivalents of sodium azide at room temperature was very successful.