Iodine → HCID 20470550, compound

Participants

Reaction Conditions

Reaction Steps

Into a 300 ml three-neck flask were added 4-(β-methyloxyethyl) biphenyl (34 g, 0.16 mol), acetic acid (112 ml), water (30 ml), iodic acid (6.8 g, 0.0384 mol), iodine (17.9 g, 0.0704 mol), carbon tetrachloride (13 ml) and conc. sulfuric acid (4.8 ml). The mixture was warmed by a mantle heater with stirring, and reaction was carried out under reflux at 83° C. for 3 hours. After completion of the reaction, the reaction liquid was cooled down to 70° C., and 10% sodium thiosulfate aqueous solution (10 ml) was added to cause excess iodine to disappear. The liquid was cooled down to room temperature, and the precipitated crystals were recrystallized from ethyl ethanol (300 ml) to obtain 4'-(β-methoxyethyl)-4-iodobiphenyl (V) (30 g) having a melting point of 97°~99.4° C.

Provenance & Evidence