1,2-Ethanedithiol → HCID 178441433, compound

Participants

Reaction Steps

0.1 g(0.000169 mole) of the aldehyde compound obtained in step 11 of Example 1 and 0.024 g(0.00025 mole) of 1,2-ethanedithiol were dissolved in 5 ml of benzene and to the resulting solution was added 0.01 mg of p-toluenesulfonic acid. The resultant was refluxed for 6 hours, neutralized with aqueous NaHCO3 solution and extracted with ethyl acetate(5 ml×3). The organic layer was dried over Na2SO4, concentrated under reduced pressure and evaporated under reduced pressure (1 mmHg, 80° C.) for 5 hours to remove the residual 1,2-ethanedithiol. The resultant was recrystallized from hexane-methylene chloride to obtain 80 mg of the title compound(yield 84%).

Provenance & Evidence