Hydrochloric Acid → Benzenesulfonyl azide

Participants

Reaction Steps

26.3 g of benzenesulphonohydrazide, 100 ml of water, 21 ml of 10N hydrochloric acid and 1.3 g of Emulgator ED (a fatty alcohol/ethylene oxide addition product) are stirred for 30 minutes, 60 g of ice are added and a solution of 19.5 g of sodium nitrite in 50 ml of water is then added dropwise in the course of about 30 minutes. The batch is stirred for 30 minutes, excess nitrite is then destroyed with a small amount of sulphamic acid, and excess acid is neutralised with about 5 ml of 10N sodium hydroxide solution. An emulsion of benzenesulphonyl azide is obtained.

Provenance & Evidence