Yield:29270-47-1 53%

Reaction Conditions:

with sulfuric acid;sulfur trioxide;iodine at 120; for 1.33333 h;

Steps:

1,2-diiodo-4,5-dinitrobenzene

Iodine (3,5 g) was dissolved in oleum (10 mL of 20 % solution of SO3 in H2SO4) and heated at 120 °C for 20 min. o-Dinitrobenzene (2.27 g, 13.5 mmol) was added. The resulting mixture was heated at 120 °C for 80 min. The reaction mixture was then poured into 500 mL of water with ice and NaOH was added until the solution was alkaline. It was extracted with chloroform (3x50 mL), combined organic phases were washed with saturated Na2S2O3 solution (100 mL) and water (100 mL) and dried over MgSO4, filtered and concentrated to dryness. Recrystallization from EtOH/H2O gave 1,2-diiodo-4,5-dinitrobenzene.

References:

Maciejewska, Agnieszka Monika;Paprocki, Daniel;Poznański, Jaros?aw;Speina, El?bieta;Winiewska‐szajewska, Maria [Molecules,2021,vol. 26,# 11] Location in patent:supporting information