Trifluoroacetic acid → HCID 58508651, compound

Participants

Reaction Conditions

Reaction Steps

A trifluoroacetic acid (3.0 mL) solution of the obtained methyl 2-(2-acetoxy-5-methoxybenzamido)-4-(2-((tert-butoxycarbonyl)(methyl)amino)phenyl)benzoate was stirred at room temperature for 1 hour and 40 minutes. The solvent was evaporated under reduced pressure, and toluene was added to the residue. The solvent was evaporated under reduced pressure, and dioxane (3.0 mL) and a 4 mol/L aqueous solution of sodium hydroxide (0.25 mL) were added to the obtained residue, followed by stirring at 50 to 55° C. for 1 hour and 30 minutes and then at 55 to 60° C. for 2 hours and 30 minutes. The reaction mixture was cooled to room temperature, and water added thereto. After adjusting the pH to 7.0 with 1 mol/L hydrochloric acid, the solvent was evaporated under reduced pressure. Water was added to the obtained residue, and the solid substance was collected by filtration to obtain 0.025 g of 2-(2-hydroxy-5-methoxybenzamido)-4-(2-(methylamino)phenyl)benzoic acid as a white solid.

Provenance & Evidence