Pinacol boronic ester substituted phenol underwent the SuEFx reaction to give 3wt in 71% yield (3u). Sterically hindered substrates 1o and 1t reacted with SO2F2 to afford the corresponding fluorosulfates 3o and 3t in 81% and 64% yields, respectively. 6hydroxyindole and pyridinol performed well yielding the corresponding heteroaryl fluorosulfates in good yields (3y and 3z). Interestingly, when 1,3-benzenediol 1h was used for the reaction, the corresponding fluorosulfate 3ah was formed in 85% yield, which is a very useful substrate in the synthesis of polysulfates. It is noteworthy that many natural phenols, such as (+)-δ-tocopherol， D-tyrosine，deoxyarbutin，maltol and so on，were proven to be very good reactants, furnishing the corresponding fluorosulfates in high yields (3ab-3ah). To explore the synthetic utility of this organocatalytic protocol, gram-scale experiments were conducted (Scheme 1). The desired aryl fluorosulfate 3a was isolated in 1.245 g, 98% yield (eq. 1). The sterically hindered fluorosulfate 3x can also be obtained in 0.857g a and 65% yield (eq. 2). novel method features extreme mild conditions, generally high reaction yields and easy scalability. Further studies on a broader substrate scope and the applications of this organocatalytic approach are currently underway in our laboratory.