Mucochloric Acid → HCID 13772910, compound

Participants

Reaction Steps

A mixture of 2.46 g (9.00 mmol) of N-(5-amino-1,2,4-triazol-3-yl)-2-chlorobenzenesulfonamide and 1.67 g (9.90 mmol) of mucochloric acid in 20 ml of DMF was heated to reflux for 16.5 hours. After cooling to room temperature, the solvent was removed by evaporation at reduced pressure and the residue was treated with 20 ml of 0.5N NaOH. After stirring vigorously for ~30 minutes the mixture was filtered through celite and the filtrate was acidified with 2N HCl. The solid which separated was collected by filtration, washed with water and recrystallized from acetic acid--water to yield 0.70 g (23 percent) of the desired product as a light brown solid, mp 285.5°-260.5° C. IR and 1H NMR spectra were in agreement with the assigned structure.

Provenance & Evidence