Abstract A simple method for ammonium persulfate mediated oxidative C(sp 3 )−H amination of azoles has been reported under mild conditions. Various azoles such as 1H‐benzotriazole, 1 H ‐1,2,3‐triazole, 2 H ‐tetrazole, 1 H ‐pyrazole and 1H‐indazole are successfully employed for coupling with tetrahydrofuran to give the products hemiaminal ethers with moderate to excellent yields. Furthermore, the C(sp 3 )−H bonds α to S, N and benzylic are also tolerated in this reaction.