Synthesis Example 1 Synthesis of 1,3,5-trichloro-2,4,6-triiodobenzene (Scheme 3-(7)) [show image] In a 100 mL three-necked flask, 1,3,5-trichlorobenzene (5.0 g, 27.6 mmol), iodine (40.3 g, 31.8 mmol), and 98% concentrated sulfuric acid (75 mL) were added, and heated and refluxed for 72 hours at 140 °C. Upon completion of the reaction, the reaction mixture was washed sequentially with aqueous sodium bisulfite, saturated aqueous sodium bicarbonate and deionized water, followed by drying. The crude product was dissolved in tetrahydrofuran (THF) and purified by recrystallization to give colorless needle-like crystals (14.3 g, 93% yield). Mass spectrum (70 eV, EI) m/z = 558 (M+); melting point > 300°C (determined in a sealed tube).
