Introduction: Most of carbonyl thioureas have been synthesized from the reaction of carbonyl isothiocyanate with amine compound in acetone. Only a few of them have been synthesized from diamine compound to produced bis-carbonyl thioureas. Objective: To investigate the one-pot reaction of 2, 3, and 4-methoxybenzoyl chloride with ammonium thiocyanate and hydrazine in acetone by reflux condition. Methods: Each of the crystal compounds was analysed by X-ray crystallography. Result: Three compound of bis-thiorea derivatives, namely N, N__ampersandsignrsquo;- bis (2-methoxy-benzamidothiocarbonyl) hydrazine (1), N, N__ampersandsignrsquo;- bis (3-methoxybenzamidothiocarbonyl) - hydrazine (2), and N, N__ampersandsignrsquo; - bis (4-methoxybenzamidothiocarbonyl) hydrazine (3) were successfully synthesised by the reaction of each 2, 3, and 4-methoxybenzoyl chloride with ammonium thiocyanate and hydrazine in acetone. The structure of these compounds was studied by chemical crystallography. Conclusion: Compound 1 and 3 were crystallized in the triclinic crystal system while compound 2 was crystallized in the monoclinic crystal system. The thiourea moiety in all compounds have trans geometry and each of the hydrogens of the amide group is trans to the carbonyl group.