Methane, characterized by its high bond dissociation energy (BDE) of C-H bonds (BDE = 105 kcal/mol), presents a substantial challenge for functionalization. Despite requiring the most demanding activation conditions, methane stands out as one of the most abundant feedstock gases, making it a highly sought-after C1 building block, if it were more facile to activate at more benign reaction conditions. To tackle the functionalization of methane, a 2-hour reaction time was employed, along with the use of deuterated acetonitrile to prevent the functionalization of the reaction solvent, a method aligned with our prior work. These optimized reaction conditions successfully yielded synthetically valuable building blocks 21 to 25 in satisfactory to good yields, ranging from 27% to 76%.