The novel insecticide tetrachlorantraniliprole was synthesized utilizing 2,3,5-trichloropyridine as the starting material by a six-step route in 18% yield. The process of simultaneous oxidation and acyl chlorination was studied by in situ FTIR. The molecular structure of tetrachlorantraniliprole was identified by means of NMR, IR, MS, and X-ray diffraction analyses. The single crystal of tetrachlorantraniliprole was formed from toluene solvent, and exhibited monoclinic P2 1 /n group with crystal parameters of a = 15.3316(16) Å, b = 16.7139(16) Å, c = 19.6687(19) Å, V = 4835.2(8) Å 3 , and Z = 4. Moreover, its density = 1.605 g/m 3 , F(000) = 2328.0, µ = 2.17 mm −1 , and 26933 reflections were measured (2.992° 2θ 51.998°).

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