Synthesis, separation and structure determination of 2,3,3'‐trichlorobiphenyl (PCB 20)† and 3,3’,4‐trichlorobiphenyl (PCB35)†

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Abstract
The combined synthesis and spectrometric characterization of 2,3,3'‐trichlorobiphenyl (PCB 20) and 3,3’,4‐trichlorobiphenyl (PCB 35) is described for the first time. By a combination of highly efficient column distillation and repeated recrystallizations it was possible to isolate the two products as reference materials with a purity exceeding 99%. X‐ray analysis of crystals of 2,3,3'‐trichlorobiphenyl positively identified the substitution pattern of the biphenyl moiety by chlorine atoms. The two phenyl rings are at an angle of 52°, while the relative disposition of the chlorine atoms on both rings is closer to anti than to syn.