Hydrochloric Acid → [1~1~,2~1~:2~4~,3~1~-Terphenyl]-1~4~,3~4~-dithiol

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Reaction Steps

4,4″-dichlorosulfonyl1,1′:4′,1″-terphenyl (8.576 g, 20 mmol) synthesized in process 1-a is dissolved in tetrahydrofuran (THF) solvent (300 ml), add lithium aluminium hydride (8.586 g, 200 mmol, 10 eq.) and refluxed for 3 hours. The obtained reacted mixture is poured into ice water, and adjusted the pH to 1 or less by adding concentrated hydrochloric acid. Deposited impurity is removed by suction filtration, then washed by methylene chloride completely. After that, the filtrate is extracted by acid-base extraction (CH2Cl2, NaOH, HCl), the organic phase is dried up using magnesium sulfate and recrystalyzed. Thus, light yellowish crystal of 4,4″-dimercapto-1,1′:4′,1″-terphenyl (3.003 g, 10.2 mmol, 51%) is obtained (compound G).

Provenance & Evidence