To 146 mg (0.55 mmol) of reagent 7 stirred at room temperature in 100 mL of CC14 was added dropwise over a 5-h period a solution of 151 mg (0.50 mmol) of the impure dithiol21 (obtained above) in 100 mL of CC14. TLC (C6H6, hexanes) 2.5 h after complete addition indicated the absence of elemental sulfur and dithiol 21. The reaction mixture, after being allowed to stand overnight, was concentrated under reduced pressure to a 5-mL volume, filtered, and ...
