Next, we investigated a range of carboxylic acids in the reaction with alkene 1a. The allylic C-H oxidation reaction has a broad scope of carboxylic acids (Fig. ). Aromatic acids, including those with diverse substituents on the aryl ring and heteroaromatic acids afforded the desired allyl esters (3x-3ae) with good yields (69-88%) and high enantioselectivities (91:9-96:4 er). Aliphatic acids with different alkyl chains, alkyl rings and ketone group can undergo the reaction, and showed high enantioselectivity (3af-3am, 94:6-96:4 er). Moreover, the unsaturated cinnamic acid can also react with alkene 1a, yielding oxidative coupling product 3an with excellent enantioselectivity (98:2 er). These results demonstrated that the reaction has a broad substrate scope. Alkynes are also suitable substrates for the enantioselective oxidative coupling with carboxylic acids, producing propargyl esters . By switching the solvent from hexafluorobenzene to 1,2dichlorobenzene, changing the light wavelength from 395 nm to 365 nm, and lowering the reaction temperature to 0 °C, we successfully realized the reaction of various alkynes with acid 2a (Fig. ). All tested aryl alkynes, including those with substituents at the aryl ring and heteroarylalkynes showed reasonable yield and high enantioselectivities (5s-5v, 91:9-97:3 er). The effect of substrate alkyl chain and its ester group on the enantioselectivity of the reaction is negligible (5s-5v).