In our previous works, we demonstrated the efficacy of trimethylaluminum as a base in iron-catalyzed C-H activation reactions. The milder nucleophilicity and lower reducibility of carbon-Al bond compared 10 with Grignard reagent and organozinc reagents accounts for the high efficacy in Fe(III)-catalyzed C-H activation. However, the undesired fast C-H alkylation after ferracycle formation constraints further development of versatile C-H functionalization reactions beyond C-H methylation. We hypothesized that reducing the nucleophilicity of the alkyl aluminum reagent by quenching two of the three alkyls on aluminum may suppress the undesired further transmetallation and hence allow the ferracycle to undergo 15 insertion with an alkyne. We considered a relatively bulky alkyl may slow down Al-Fe transmetallation in comparison to AlMe3. The hypothesis prompted us to test using catechol to quench triisobutyl aluminum, Al(i-Bu)3, a commercially available aluminum reagent sold as a solution in toluene.