Trifluoroacetic acid → HCID 86687733, compound

Participants

Reaction Steps

N-(4-methoxybenzyl)-1-(2-methoxyphenyl)-4-oxo-N-(1,2,4-thiadiazol-5-yl)-3,4-dihydrophthalazine-6-sulfonamide (65.0 mg, 0.121 mmol) was dissolved in DCM (1.21 mL) and then TFA (46.7 μl, 0.607 mmol) was added. After 1 d at rt, LCMS showed mainly product. The reaction was quenched with 1 mL of saturated aqueous NaHCO3 and was concentrated. Chromatography was performed using reverse phase Isolera through a pre-packed C18 column (12 g), eluting with a gradient of 0% to 60% MeCN with 1% TFA in water with 1% TFA. Fractions containing the product were combined and concentrated. White solid precipitated out of the water. The solid was filtered off with an aid of water and dried to afford 1-(2-methoxyphenyl)-4-oxo-N-(1,2,4-thiadiazol-5-yl)-3,4-dihydrophthalazine-6-sulfonamide (11 mg, 21.8% yield). m/z (ESI) 416.0 (M+H)+.

Provenance & Evidence