Heteroatom Chemistry Volume 00, Number 0, 2012 Microwave-Assisted Synthesis of Disulfides Using Tetrathiomolybdate: A Step toward Greener Synthesis Naheed Sidiq, Mohsin Ahmad Bhat, Khaliquz Zaman Khan, and Mohammad Akbar Khuroo Department of Chemistry, University of Kashmir, Srinagar 190 006, India Received 27 July 2011; revised 23 February 2012 ABSTRACT: An eco-friendly, efficient, and rapid syn- thetic procedure for disulfides using benzyl triethyl am- monium tetrathiomolybdate through microwave irra- diation of solid support adsorbed reactants is reported. C  2012 Wiley Periodicals, Inc. Heteroatom Chem 00:1–4, 2012; View this article online at wileyonlinelibrary.com. DOI 10.1002/hc.21025 INTRODUCTION The synthesis and chemistry of disulfides continue to be an area of considerable interest among re- searchers on account of their biological role, indus- trial applications, and utility in organic synthesis [1–5]. Although a variety of methods have been devised for their synthesis, disulfides are mostly synthesized from the corresponding halides, thio- cyanates, and alcohols using tetrathiomolybdate [2,4]. This is due to advantages such as straight- forward reaction methodologies and mild reaction conditions that can be tuned green by careful and intelligent modifications in the experimental proce- dure. An appropriate choice of parameters in these steps is expected to ensure the synthesis of disul- fides through solventless and/or use of eco-friendly solvent choices and biphasic catalysis pathways. The disadvantages such as longer reaction times, opera- tional complications, and the use of volatile organic Correspondence to: Mohammad Akbar Khuroo; e-mail: khuroo .mohammadakbar@gmail.com. c  2012 Wiley Periodicals, Inc. compounds (VOCs) in this often opted procedure for disulfide synthesis have been a great challenge for environment-conscious synthetic chemists. Such challenges in synthetic organic chemistry are usually overcome through the use of unconventional reactor designs and reaction pathways that require the use of nonhazardous and eco-friendly chemicals to ensure efficient and green synthesis of desired substances. It is in this context that microwave irradiation cou- pled with solid support is receiving considerable attention in organic synthesis [6–8]. The use of mi- crowave irradiation in organic synthesis has ensured minimal or no use of VOCs, simple workup coupled with higher yields, shorter reaction times, low energy consumption, and selectivity [9–13] in certain reac- tions. In view of these facts and drawing an inspira- tion from some recent reports [14,15], we attempted the use of microwave irradiation in the synthesis of disulfides from alkyl halides and thiocyanates us- ing benzyl triethyl ammonium tetrathiomolybdate (BTATM). In the present communication, we report results from our preliminary investigations about the synthesis of disulfides through microwave irra- diation of solid-supported reactants. The main find- ing of the present communication is that the use of microwave irradiation turns the conventional syn- thetic procedure of disulfides eco-friendly, efficient, and time saving. RESULTS AND DISCUSSION Before attempting the microwave-assisted synthe- sis, we explored the stability of silica-supported as well as water-solubilized BTATM on exposure to 1