A straightforward procedure for the synthesis of (Ph[subscript 3]P)[subscript 3]CuCF[subscript 3], a robust, air-stable trifluoromethylating agent, is reported herein. This preparation can be completed in a single 3 h laboratory session and typically provides ample yields (~79--86%) and high purity (>90%). The target complex is characterized by students primarily using heteronuclear ([superscript 19]F, [superscript 31]P) NMR methods. A 30 min application experiment, using this product, has also been developed in which students are able to trifluoromethylate an aryl iodide on an NMR scale and monitor their reaction progress using [superscript 19]F NMR.