Acetohydrazide → HCID 66581078, compound

Participants

Reaction Conditions

Reaction Steps

To a solution of 3-[3-(ethoxycarbonyl)-5,5-dioxidothiochromeno[4,3-c]pyrazol-1(4H)-yl]benzoic acid (200 mg, 0.485 mmol) in EtOAc is added acetic hydrazide (35 mg, 0.485 mmol) under nitrogen. Then TEA (0.2 mL, 1.45 mmol) and propane phosphonic acid cyclic anhydride (0.7 mL, 1.2 mmol) is added to the reaction mixture at 0° C. under nitrogen. The reaction mixture is refluxed at 80° C. for 12 h after which it is diluted with EtOAC and washed with 10% aq. Na2CO3 solution. The organic layer is separated, dried over Na2SO4 and concentrated under reduced pressure. The solid residue is purified by silica gel column chromatography over (1.5% MeOH in DCM to afford the title compound. MS (ESI+): 451.2.

Provenance & Evidence