Chlorosulfonic acid → HCID 178527428, compound

Participants

Reaction Steps

Benzotriazole-4-sulphonic acid (5 g, 23 mM) was added, in portions, to chlorosulphonic acid (50 ml), whilst keeping the temperature of the acid below 0°. The resulting solution was heated at 120° overnight, cooled and carefully poured onto ice (1000 g). The solid which formed was collected by filtration, washed well with water and dried in vacuo. This material was dissolved in boiling ethyl acetate and decolorized using a small quantity of charcoal. The product crystallized from the ethyl acetate solution after petroleum ether (40° to 60°) was added, as a white solid (3.94 g, 72 percent), m.p. 173° to 175° (uncorr).

Provenance & Evidence