Abstract Thirty‐three crystalline urethanes were prepared by the condensation of the new reagent, 3:5‐dinitro‐4‐methyl‐benzazide, in boiling ligroin solution with various phenols. The very high yields of the 3:5‐dinitro‐4‐methylphenyl‐urethanes obtained from the reaction and the excellent properties of these derivatives, indicated that 3:5‐dinitro‐4‐methyl‐benzazide is an excellent micro‐reagent for the identification of phenols.