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A method is described for the isolation of pure phenanthro[4,5‐bcd] thiophene (4) from a sulfur‐bridging reaction mixture, also containing phenanthrene (3) and elemental sulfur, by selective oxidation of 4 to the sulfoxide (5) by means of iodobenzene dichloride, chromato‐graphic separation of 5 on silica gel, and finally reduction of 5 back to 4 by means of sodium bis(methoxyethoxy)aluminum hydride in 25% overall yield from 3.
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Klemm et al. (1976) studied this question.
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