in Wiley Online Library (wileyonlinelibrary.com).In this article, an efficient, environmentally benign, one-pot and simple synthesis of 2-aryl/heteroarylbenzothiazoles by the reaction of 2-aminothiophenol and aryl/heteroaryl aldehydes mediated by hypervalent iodine (III) reagents under solvent-free condition at room temperature is demonstrated. All the reactions were carried out by grinding the reactants (2-aminothiophenol and aryl/heteroaryl aldehydes) with hypervalent iodine (III) reagents in a mortar with pestle. Phenyliodine bistrifluoroacetate act as an efficient oxidizing reagent in comparison to iodobenzene diacetate in term of reaction time but yields are comparative. The advantages of this protocol are the one-step procedure, mild reaction conditions, high yields of the products, and no side reactions. CDCl 3 ): δ 3.87 (s, 3H), 6.98-7.02 (m, 2H), 7.30-7.36 (m, 2H), 7.44-7.50 (m, 3H), 7.67-7.69 (m, 2H), 7.76-7.78 (m, 1H), 7.81-7.83 (m, 2H), 8.02 (d, J = 8.0 Hz, 1H), 8.66 (s, 1H). Anal. Calcd. for C 23 H