Dihydroisocoumarins are an important class of naturally occurring, biologically active δ-lactones. Numbers of such dihydroisocoumarins have varied uses, ranging from sweetening agents to bactericides, antimalarial, antituberculous, antifungal, antiulcerogenic, and antitumor. 1,2 Owing to its natural occurrence and important activities, the synthesis and crystal structure determination of dihydroisocoumarins have remained active subjects of interest. However, only little attention has been paid to 3,3-disubstituted dihydroisocoumarins. Therefore, as a part of our program on crystal structure analysis of a variety of dihydroisocoumarins 3 and with a goal to synthesize a noble 3,3-disubstituted dihydroisocoumarin system, the present compound was synthesized. N-Methyl-o-toluamide (0.0134 mol) was dissolved in dry THF (50 mL) and metalated with n-BuLi (prepared from 1.3 g lithium and 7.0 mL n-BuBr in dry ether). The resultant metalated solution was stirred for 30 min at room temperature. It was then cooled to-15˚C and an ethereal solution of desoxy benzoin (0.07 mol in 25 mL dry ether) was added during 10 min. The reaction mixture was stirred for 30 min at this temperature, and then further stirred at room temperature for 1 h. A work up of the reaction was carried out using a literature procedure 4 described for such condensation. The reaction afforded 3-benzyl-3-phenyl-3,4-dihydroisocoumarin (Fig. 1) as crystalline solid (yield: 2.1 g, m.p.: 105˚C).