AbstractA simple method for ammonium persulfate mediated oxidative C(sp3)−H amination of azoles has been reported under mild conditions. Various azoles such as 1H‐benzotriazole, 1H‐1,2,3‐triazole, 2H‐tetrazole, 1H‐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(sp3)−H bonds α to S, N and benzylic are also tolerated in this reaction.