4,5-DIBROMO-1H-1,2,3-TRIAZOLE synthesis

Yield: 98.7%

Reaction Conditions:

with bromine in water at 50; for 3.33333 h;Inert atmosphere;Schlenk technique;

Steps:

4,5-Dibromo-1H-1,2,3-triazole:
To a 500 mL Erlenmeyer flask, 1,2,3-triazole (20.0 g, 290mmol) and 200 mL of H2O were added. To a stirring solution, Br2 (20.0 mL, 389 mmol) wasslowly added over 20 minutes. This solution was then heated to 50 °C and stirred for 3 h duringwhich a precipitate formed. The precipitate was collected by vacuum filtration and washed witha copious amount of water. To the filtrate, another 20.0 mL (389 mmol) of Br2 was added andstirred for an additional 18 h. The formed precipitate was then collected via vacuum filtrationand washed with water (~100 m). Another 10.0 mL (194 mmol) of Br2 was then added to thefiltrate and stirred for another 18 h. The last of the precipitate was collected and washed withwater (~100 mL). All of the product was then dried in a vacuum oven producing an off-whitesolid (64.85 g, 98.7%). This product was carried on without any further purification or analysis.

References:

Albright, Savannah G.;Ali, Bakr;Chapman, Hayley A.;Cheng, Yijie;Cusic, Rachel M.;Friese, Seth J.;Hartlove, Nathan B.;Labb, Samantha A.;Marr, Alissa N.;Masteran, Conner J.;Timmons, Miranda [Synlett,2020,vol. 31,# 14,p. 1384 - 1388] Location in patent:supporting information