Potassium Carbonate → HCID 23353989, compound

Participants

Reaction Steps

To a solution of 3 g of 8-acetoxyacetyl-4,4a,5,6-tetrahydro-2-(4methylphenyl)thieno-[2,3-h]cinnolin-3(2H)-one in 30 ml of trifluoroacetic acid was added 2.7 ml of triethylsilane and the mixture was stirred at room temperature for 24 hours. The mixture was poured into ice-cold water, neutrallized with potassium carbonate and then extracted with chloroform. The extract was washed with brine, dried over anhydrous magnesium sulfate and concentrated in vacuo. The residue was chromatographed on a silica gel (SiO2 :100 g) column using chloroform as an eluent. The resulting solid was recrystallized from a mixed solvent of ethyl acetate and hexane to give 2.0 g of 8-(2-acetoxyethyl)-4,4a,5,6-tetrahydro-2-(4-methylphenyl)thieno-[2,3-h]cinnolin-3(2H)-one as a white powder, melting at 73°-75° C.

Provenance & Evidence