Sulfuric Acid → HCID 57667966, compound

Participants

Reaction Steps

To a suspension of water 6.0 mL, acetic acid 10 mL and concentrated sulfuric acid 0.95 mL of 2-amino-4-phenoxybenzoic acid 2.0 g was added water 2.0 mL solution of sodium nitrite 0.66 g at 4° C., and it was stirred at same temperature for 30 minutes. The reaction mixture was added dropwise to water 30 mL solution of potassium iodide 3.2 g at same temperature, and it was stirred at room temperature for 3 hours. Ethyl acetate was added to the reaction mixture. The organic layer was separated and collected,dried over anhydrous magnesium sulfate, and the solvent was removed under reduced pressure. The obtained residue was refined by silica gel column chromatography [eluent; hexane:ethyl acetate:acetic acid=80:20:1] to give 2-iodo-4-phenoxybenzoic acid 1.6 g of red solid.

Provenance & Evidence