HCID 19759911, compound → HCID 19759872, compound

Participants

Reaction Conditions

Reaction Steps

4,5-Dihydrothieno[2,3-b]thiophene-2-carboxylic acid (88.3 g, 0.474 mol) was added to a solution of Oxone® (730 g, 1.18 mol) in water (3.0 L), and the resulting suspension heated on a steam bath for 1 hour. During this time the solids dissolved to give a clear yellow solution. The reaction was cooled to 60° C. and filtered. The filtrate was extracted four times with ethyl acetate (6 L total) and the combined extracts washed with saturated brine and dried over magnesium sulfate. The solution was filtered and concentrated in vacuo to give the title compound as a yellow solid (70 g, 68%). Recrystallization from dichloroethane gave an off-white powder, mp=227°-230° C. Anal. Calc. for C7H6O4S2 : C, 38.52; H, 2.77. Found: C, 38.53; H, 2.61.

Provenance & Evidence