Sulfuric Acid → HCID 59392440, compound

Participants

Reaction Conditions

Reaction Steps

265 ml of conc. sulfuric acid are initially introduced in an argon-flushed 3-necked flask and cooled to 0° C. 124.2 g (0.705 mol, 3 eq.) of ascorbic acid and subsequently 60 g of 3-benzotriazol-2-yl-4-hydroxybenzoic acid (0.235 mol, 1 eq.) are added in portions. 73.7 ml of oleum (sulfuric acid containing 65% of SO3) are then added dropwise. After a reaction time of 5 hrs. at 45° C., the reaction solution is poured onto 1000 g of ice, saturated with 200 g of sodium chloride and extracted 3× with 1000 ml of ethyl methyl ketone. The combined org. phases are extracted with 500 ml of sat. NaCl solution, dried over sodium sulfate, and the solvent is removed in vacuo. Crystallisation from ethyl acetate gives the product as a white solid.

Provenance & Evidence