Flash Communication: A Glovebox-Friendly Synthesis of CrCl 3 (THF) 3 from CrCl 2 and Trityl Chloride

mer-CrCl3(THF)3 is a useful and labile precursor for Cr(III) organometallic chemistry, but the commercial material is costly and sometimes poorly defined, whereas existing synthetic routes to the complex rely on corrosive reagents, prolonged reaction times, or elaborate experimental setups which are impractical for glovebox work. Herein we present a facile, mild, and glovebox-friendly synthesis of mer-CrCl3(THF)3 as purple crystals from CrCl2 using solid trityl chloride as a chlorinating agent in THF. The reaction proceeds in 2.5 h at 75 °C or overnight at room temperature, directly yielding crystalline mer-CrCl3(THF)3 in 70–84% yield with minimal workup; the only organic byproduct is Gomberg’s dimer, Ph3CC6H5CPh2, which is readily removed by hexane washings. This operationally simple method avoids corrosive, toxic, and volatile reagents, minimizes waste, and provides reliable and ready access to mer-CrCl3(THF)3. The THF adduct undergoes a clean ligand substitution reaction with Na(pyrNdipp) to afford the structurally characterized Cr(III) complex Cr(pyrNdipp)2Cl(THF), illustrating the synthetic utility of the material.